Author: Jessica.F

In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. 5003-71-4, name is 3-Bromopropan-1-amine hydrobromide belongs to bromides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Quality Control of 3-Bromopropan-1-amine hydrobromide

To 3-bromopropylamine hydrobromide (139.32 g, 636.40 mmol) was added a solution of di-tert-butyl dicarbonate (112.46 g, 510.13 mmol) in MIBK (800 mL) and 2.5 M sodium hydroxide (310 mL). The resulting mixture was stirred for 1 hour at room temperature. The reaction was monitored by TLC (9:1 isohexane: ethyl acetate, potassium permanganate stain). Water (345 mL) was added and the mixture stirred for 10 minutes. The phases were separated and the lower (aqueous) phase discarded. To the retained organic phase was added 3-benzyl-9- oxa-3,7-diazabicyclo[3.3.1]nonane dihydrochloride (148.43 g, 509.68 mmol; .; see WO 02/083690) and 2.5 M sodium hydroxide (660 mL). This mixture was heated at 65C for 7 hours. At 650C, the phases were separated and the lower (aqueous) phase discarded. The organic phase was re-heated to 650C and extracted with 10% w/w aqueous citric acid (562 mL). The phases were separated and the upper (organic) phase discarded. To the resulting aqueous phase was added MIBK (800 mL) and 5 M sodium hydroxide (230 mL) containing approximately 10% w/v EPO sodium chloride (22.84 g). The resulting mixture was stirred at room temperature for 15 minutes. The phases were separated and the lower (aqueous) phase discarded. The organic phase was azeo-dried by removal of solvent (300 mL) by distillation under reduced pressure (keeping the temperature below 7O0C). The mixture was clarified by filtration whilst still hot and the residue washed with MIBK (115 mL). The temperature was adjusted to 6O0C and a solution of purified (see J. Am. Pharm. Assoc. 239-241 (1949)) 4-chlorobenzenesulfonic acid (99.24 g, 515.20 mrnol) in MIBK (225 mL) was added over 90 minutes. The reaction mixture was then cooled to room temperature causing the product to crystallize from solution. The mixture was cooled to 5C, the product was collected by filtration and the cake washed with MIBK (225 mL). The product was dried as far as possible on the filter, then oven dried in vacuo (50C, 24 h) to give the title compound as a white solid (257.44 g, 453.13 mmol, 89%). 1H NMR (300 MHz, DMSO-d6) delta 7.61 (d, J= 8.7 Hz, 2H), 7.46 – 7.35 (m, 7H), 7.10 (t, J= 5.7 Hz, IH), 4.15 (s, 2H), 3.70 (s, 2H), 3.40 (d, J= 12.1 Hz, 3H), 3.07 (d, J= 11.9 Hz, 4H), 2.97 (q, J= 6.3 Hz, 2H), 2.84 (t, J= 7.1 Hz, 2H), 2.76 (d, J= 11.9 Hz, 2H), 1.70 (quintet, J= 6.7 Hz, 2H), 1.45 (s, 9H).

The synthetic route of 5003-71-4 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; ASTRAZENECA AB; WO2006/137770; (2006); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps, and cheap raw materials. 766-46-1, name is 2′-Bromophenylacetylene, A new synthetic method of this compound is introduced below., Application In Synthesis of 2′-Bromophenylacetylene

General procedure: To the mixture of phenylacetylene (1 mmol), water (3.0 mL),silver perfluorooctanesulfonate (5 mol%) and perfluorooctane sulfonateacid (2 mol%) was added. The mixture was stirred at 100 Cfor 8 h. The solution was extracted with n-hexane (diethyl ether)(3 5 mL), the combined extract was dried with anhydrous MgSO4. The rest of the solution was used for the next cycle of reaction. Theextraction solvent was removed and the crude product was separatedby column chromatography to give the pure sample.

The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.

Reference:
Article; Dong, Qizhi; Li, Ningbo; Qiu, Renhua; Wang, Jinying; Guo, Cancheng; Xu, Xinhua; Journal of Organometallic Chemistry; vol. 799-800; (2015); p. 122 – 127;,
Bromide – Wikipedia,
bromide – Wiktionary

Application of 58971-11-2, The chemical industry reduces the impact on the environment during synthesis 58971-11-2, name is 3-Bromophenethylamine, I believe this compound will play a more active role in future production and life.

General procedure: To compound 5, 6 or 7 (1 equiv) and the appropriate alkylamine(1.3 equiv) in anhydrous DMF (10 mL/mmol) were added DIEA (3equiv) and PyBOP (1 equiv), and the reaction mixturewas stirred atroom temperature under argon. When the reaction was complete(2 h – 4 h), the solvents were removed under reduced pressure togive a residue that was taken up in CH2Cl2. The solution waswashed with saturated aqueous NaHCO3, then water. The organiclayer was dried over Na2SO4 and then evaporated in vacuo. Purificationby flash chromatography afforded the corresponding amidederivatives 8, 9 or 10 (yield: 40-76%).

In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles, 3-Bromophenethylamine, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Paoletti, Julie; Assairi, Liliane; Gelin, Muriel; Huteau, Valerie; Nahori, Marie-Anne; Dussurget, Olivier; Labesse, Gilles; Pochet, Sylvie; European Journal of Medicinal Chemistry; vol. 124; (2016); p. 1041 – 1056;,
Bromide – Wikipedia,
bromide – Wiktionary

Adding a certain compound to certain chemical reactions, such as: 3972-64-3, name is 1-Bromo-3-(tert-butyl)benzene, belongs to bromides-buliding-blocks compound, can increase the reaction rate and produce products with better performance than those obtained under traditional synthetic methods. Here is a downstream synthesis route of the compound 3972-64-3, Formula: C10H13Br

Step 1: Synthesis of 3-tert-butylphenylboronic acid To a solution of dry THF (10 mL) was added magnesium (1.25 g, 52 mmol), 3-t-butyl bromobenzene (2.0 g, 9.4 mmol) and a crystal of iodine. The reaction was first heated slightly until the reaction started and then removed. The remaining 3-t-butyl bromobenzene (8.0 g, 37.7 mmol) was added via an addition funnel until the spontaneous refluxing stopped. The reaction mixture was heated to reflux for 2 hours. The Grignard was transferred via a syringe into a cooled solution (-40° C.) of trimethyl borate dissolved in THF and added over a 10 minute period. The reaction mixture was warmed to room temperature overnight. Ethyl acetate and distilled water were added to the reaction mixture and the layers separated. The organics were washed with brine and dried over magnesium sulfate. The solvent was concentrated and the product purified by a silica gel column using 10percent ethyl acetate and hexanes as the eluants to give 3-t-butylphenyl boronic acid (4.0 g, 46percent yield) as a white solid. The product was confirmed by GCMS and was used directly in the next step.

In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles, 1-Bromo-3-(tert-butyl)benzene, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Universal Display Corporation; EP2243785; (2010); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

These common heterocyclic compound, 1559-88-2, name is 3-Bromo-1,2,4,5-tetrafluorobenzene, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route. Application In Synthesis of 3-Bromo-1,2,4,5-tetrafluorobenzene

Example H 4-Bromo-2,3,5,6-tetrafluorophenylsulfonyl Chloride. The title compound was synthesised from 1-bromo-2,3,5,6-tetrafluorobenzene by a method similar to that used in Example F. MS (EI): 328 (20, M+), 293 (70), 229 (50), 148 (100).

The synthetic route of 3-Bromo-1,2,4,5-tetrafluorobenzene has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Tularik INC; US6284923; (2001); B1;,
Bromide – Wikipedia,
bromide – Wiktionary

Electric Literature of 138526-69-9, The chemical industry reduces the impact on the environment during synthesis 138526-69-9, name is 1-Bromo-3,4,5-trifluorobenzene, I believe this compound will play a more active role in future production and life.

General procedure: In a typical experiment a dry and argonflushed50-mL Schlenk tube, equipped with a magnetic stirring bar, was charged with therespective fluorinated bromobenzene derivative (0.5 mmol, 88 mg for monosubstituted, 97 mgfor disubstituted and 105 mg for trisubstituted derivatives) and 3 mol% of the respective catalystdissolved in 15 ml of THF ([FeCl2(dppe)]: 7.9 mg, [FeCl2(dppp)]: 8.1 mg, [NiCl2(dppm)]: 7.7mg, [NiCl2(dppe)]: 7.9 mg, [NiCl2(dppp)]: 8.1 mg, [PdCl2(dppm)]: 8.4 mg, [PdCl2(dppe)]: 8.6mg, [PdCl2(dppp)]: 8.8 mg). The solution was stirred for 5 min, then cyclohexyl magnesiumbromide or the respective LiCl or LiBr adduct (0.8 mmol, 4 ml of a 0.2M Grignard reagent) wasquickly added to the reaction mixture and vigorous stirring at room temperature was continuedfor 24 hours. After hydrolysis with diluted hydrochloric acid, the organic layer and ether extractsfrom the aqueous layer were combined, washed with water and saturated NaCl solution, driedover MgSO4 and filtrated through a pad of silica. Concentration under reduced pressure followedby column chromatography (hexane : diethyl ether, v/v 100 : 1) afforded the respective coupling products as light yellow oily compounds

In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles, 1-Bromo-3,4,5-trifluorobenzene, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Dahadha, Adnan; Imhof, Wolfgang; ARKIVOC; vol. 2013; 4; (2013); p. 200 – 216;,
Bromide – Wikipedia,
bromide – Wiktionary

Related Products of 1435-52-5, As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 1435-52-5 name is 1,4-Dibromo-2-fluorobenzene, This compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below.

General procedure: 6.13 1-(4′-Ethylphenyl)-4-(4″-ethylphenyl)-2-fluorobenzene (7m): Starting with 6 (200 mg, 0.79 mmol), Cs2CO3 (385 mg, 1.81 mmol), Pd(PPh3)4 (3 molpercent), 4-ethylphenylboronic acid (237 mg, 1.58 mmol) and 1,4-dioxane (4 mL), 7m was isolated as a colorless solid (195 mg, 81percent). Mp 111 °C. 1H NMR (300 MHz, CDCl3): delta = 1.20 (t, J = 15.2 Hz, 7.5 Hz, 3H, CH3), 1.22 (t, J = 15.2 Hz, 7.5 Hz, 3H, CH3), 2.62 (t, J = 15.1 Hz, 7.4 Hz, 4H, 2CH2), 7.19-7.22 (m, 4H, ArH), 7.27-7.40 (m, 3H, ArH), 7.42-7.47 (m, 4H, ArH). 13C NMR (75 MHz, CDCl3): delta = 15.6 (d, J = 2.2 Hz, 2CH3), 28.6 (d, J = 5.5 Hz, 2CH2), 114.4 (CH), 114.5 (CH), 122.7 (d, J = 4.0 Hz, CH), 126.9 (2CH), 127.4 (d, J = 13.8 Hz, C), 128. (2CH), 128.5 (2CH), 128.9 (d, J = 4.0 Hz, CH), 130.8 (d, J = 4.0 Hz, CH), 132.9 (C), 136.9 (C), 141.9 (d, J = 8.3 Hz, C), 143.9 (d, J = 20.9 Hz, CH), 160.1 (d, JCF = 247.0 Hz, CF). 19F NMR (282 MHz, CDCl3): delta = -117.24 (CF). IR (ATR, cm-1): , 2963 (w), 2873 (w), 2361 (w), 1609 (w), 1544 (w), 1485 (w), 1428 (w), 1394 (w), 1295 (w), 1260 (w), 1180 (w), 1135 (w), 1050 (w), 1004 (w), 970 (w), 889 (w), 814 (w), 728 (w), 696 (w), 641 (w), 582 (w), 499 (w), 417 (w) cm-1. GC-MS (EI, 70 eV): m/z (percent) = 304 (100) [M]+, 290 (18), 289 (80), 274 (21), 137 (17). HRMS (ESI) calcd. for C22H22F [M + H]+: 305.17001; found 305.16948. Anal. calcd. for C21H17FO2: C,86.85. H, 6.91. Found: C, 86.82. H, 6.88.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 1,4-Dibromo-2-fluorobenzene, and friends who are interested can also refer to it.

Reference:
Article; Sharif, Muhammad; Maalik, Aneela; Reimann, Sebastian; Feist, Holger; Iqbal, Jamshed; Patonay, Tama?s; Villinger, Alexander; Langer, Peter; Journal of Fluorine Chemistry; vol. 146; (2013); p. 19 – 36;,
Bromide – Wikipedia,
bromide – Wiktionary

In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. 57951-72-1, name is 1-Bromo-2-cyclopropylethyne belongs to bromides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. HPLC of Formula: C5H5Br

To a solution of (bromoethynyl)cyclopropane (60 g, 414 mmol) in piperidine (345 ml) at 0 C. was added ethynyltrimethylsilane (44.7 g, 455 mmol) and CuI (7.88 g, 41.4 mmol). The solution was then stirred at rt for 2 hours. The reaction was quenched by adding sat. aq. NH4Cl solution and then extracted with TBME. The organic layer was washed with water, brine, dried over MgSO4 and concentrated. The crude material was purified by silica gel column chromatography, heptane as eluant to give product (42 g, 62% yield). 1H NMR (400 MHz, CDCl3) 0.13-0.24 (m, 9H) 0.72-0.91 (m, 4H) 1.25-1.36 (m, 1H)

The synthetic route of 57951-72-1 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Novartis AG; FU, Jiping; JIANG, Siyi; KORDIKOWSKI, Andreas; SWEENEY, Zachary Kevin; (21 pag.)US2017/355684; (2017); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Each compound has different characteristics, and only by selecting the characteristics of the compound suitable for a specific situation can the compound be applied on a large scale. 102169-44-8, name is 4-Bromo-5-methylbenzene-1,2-diamine, This compound has unique chemical properties. The synthetic route is as follows., category: bromides-buliding-blocks

4-bromo-5-fluorobenzene-1,2-diamine (500 mg, 2.44 mmol), 1-(cyclopropylmethyl)-4-(4, 4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)-1H-pyrazole (see Intermediate 01-06; 1.21 g, 4.88 mmol), an aq. solution of sodium carbonate (3.0 ml, 2.0 M, 6.1 mmol) and 1 ,1 ‘-bis(diphenylphosphino)ferrocene-palladium(ll)dichloride dichloromethane complex (49.8 mg, 61.0 _) were stirred in THF (1 1 ml) overnight at 60C. The mixture was diluted with water and extracted three times with dichloromethane. The combined organic phases were dried over a silicone filter and concentrated under reduced pressure. The crude mixture was purified by flash chromatography on silica gel to give 350 mg (90 % purity, 52 % yield) of the title compound. LC-MS (Method 2): Rt = 0.84 min; MS (ESIpos): m/z = 247 [M+H]+ 1H-NMR (400MHz, DMSO-d6): _ [ppm]= 0.32 – 0.39 (m, 2H), 0.49 – 0.56 (m, 2H), 1.24 (s, 1H), 3.96 (d, 2H), 4.26 – 4.38 (m, 2H), 4.76 (s, 2H), 6.35 (d, 1H), 6.71 (d, 1H), 7.57 (dd, 1H), 7.84 (dd, 1H).

Chemical properties determine the actual use. Each compound has specific chemical properties and uses. We look forward to more synthetic routes in the future to expand reaction routes of 102169-44-8.

Reference:
Patent; BAYER PHARMA AKTIENGESELLSCHAFT; LEFRANC, Julien; MENGEL, Anne; SCHULZE, Volker; CHRIST, Clara; PRINZ, Florian; WENGNER, Antje, Margret; STOeCKIGT, Detlef; BOeMER, Ulf; BADER, Benjamin; (288 pag.)WO2017/207534; (2017); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Related Products of 1647-26-3, The chemical industry reduces the impact on the environment during synthesis 1647-26-3, name is 1-Bromo-2-cyclohexylethane, I believe this compound will play a more active role in future production and life.

General procedure: A mixture of 3-methyl-hypoxanthine (0.59 mmol, 89 mg) and anhydrous potassium carbonate (amounts, see Tables in the article) in dry DMSO (23 mL) was stirred under N2 at ambient temperature for 1 h. Alkyl halide (amounts, see Tables in the article) in dry DMSO (5 mL) was added over 5 min by a syringe pump (rate 60 mL/h). The reaction mixture was stirred for at ambient temperature for the time given in the article. The mixture was filtered, the filtrate concentrated in vacuo and the residue was purified by flash chromatography on SiO2. In cases where the product was not completely pure after chromatography, the material isolated was cooled to 5 C in a 50 mL round bottom flask, and stirred moderately for 2 h in distilled hexane (50 mL). The solid was allowed to settle (1 h) and most of the hexane was removed carefully by a pipette, leaving a small volume, so as not to remove the fine particles of product at the bottom. The remaining hexane was removed by concentration in vacuo.

In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles, 1-Bromo-2-cyclohexylethane, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Chamgordani, Elahe Jafari; Paulsen, Jan; Gundersen, Lise-Lotte; Tetrahedron Letters; vol. 57; 44; (2016); p. 4926 – 4929;,
Bromide – Wikipedia,
bromide – Wiktionary