Tag: M.W=200-300

Reference of 345965-54-0, In the chemical reaction process, reaction time, type of solvent, can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product. An updated downstream synthesis route of 345965-54-0 as follows.

A solution of 1-(4-bromophenyl)-cyclopropylamine (Intermediate 116,244.0 mg, 1.15 mmols) and benzyl bromide (255.0 mg, 1.50 mmols) in 4 mL DMF was stirred at 85 C. for 6 hours, cooled to room temperature and stirred overnight. The solution was diluted with H2O and the pH adjusted to 8-9 with aqueous NaOH. The solution was extracted with EtOAc and the combined organic layers were washed with H2O and saturated aqueous NaCl, dried (MgSO4) and concentrated under reduced pressure. Column chromatography (5-10% EtOAc-Hexanes) afforded 110 mg (32%) of the N-benzyl amine. 1H NMR (CDCl3) delta: 7.48 (2H, d, J=8.4 Hz), 7.30-7.23 (7H, m), 3.68 (2H, s), 1.07 (2H, m), 0.93 (2H, m); and 100 mg (22%) of the N,N-dibenzyl amine, 1H NMR (CDCl3) delta: 7.55 (2H, d, J=8.3 Hz), 7.40-7.19 (12H, m), 3.61 (4H, s), 0.87 (2H, m), 0.71 (2H, m).

According to the analysis of related databases, 345965-54-0, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Allergan Sales, Inc.; US6252090; (2001); B1;,
Bromide – Wikipedia,
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Reference of 393-37-3, 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. 393-37-3, name is 5-Bromo-2-fluorobenzotrifluoride, This compound has unique chemical properties. The synthetic route is as follows.

Compound 28 (200 mg, 0 . 823mmol), compound 29 (86.34 mg, 0 . 549mmol) and K2CO3(227.63 mg, 1 . 647mmol) to 25 ml in two neck bottles, the oil pump and the gas is removed using argon saturated, syringe injection 3ml THF and 1ml H2O, then re-used to remove saturated with argon gas and in the bottle. Slowly adding PdCl2(PPh3)2(38 mg, 0 . 0549mmol), water pump for removing saturated with argon gas and in the bottle. The temperature is increased to 70 C, stirring reflux 2h. The reaction solution with ethyl acetate extraction 3 time, combined with the organic layer, anhydrous Na2SO4drying, concentration. Column chromatography PE_EA= 100:1 to 120 mg white solid 3, yield 53%

The chemical industry reduces the impact on the environment during synthesis 5-Bromo-2-fluorobenzotrifluoride. I believe this compound will play a more active role in future production and life.

Reference:
Patent; SICHUAN BAILI PHARMACEUTICAL CO LTD; WU, YONG; ZHU, YI; HAI, LI; LI, JIE; YU, YONGGUO; LIU, WEIJIA; (26 pag.)CN103804312; (2016); B;,
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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. 608-30-0, name is 2,6-Dibromoaniline belongs to bromides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Computed Properties of C6H5Br2N

General procedure: A flask equipped with a septum and a stirring bar was charged with aniline derivative (2.00 g, 1.00 equiv). The flask was closed andTHF (5 mL) was added by using a syringe under an argon atmosphere.The solution was cooled to -20 C and BF3*OEt2(1.50 equiv) was added. Isoamyl nitrite (1.50 equiv) was then slowly added under vigorous stirring and the solution was stirred for 2 hat this temperature. The precipitate was filtered off and washed withice-cold Et2O. Without further isolation, the precipitate was then poured (with MeCN wash) into a freshly a prepared solution containing i-Pr2NH (3.00 equiv) in a mixture of THF-pyridine (9:1, 10 mL) at -20 C. The solution was stirred and allowed to warm slowly to r.t. for an additional 16 h. The reaction was then quenched with sat. NH4Cl solution, the aqueous phase was extracted twice with EtOAc and the organic layer was dried over MgSO4. The solvent was removed in vacuum and the crude product was purified by flash column chromatography (silica gel).

The synthetic route of 608-30-0 has been constantly updated, and we look forward to future research findings.

Reference:
Review; Hafner, Andreas; Hussal, Christoph; Braese, Stefan; Synthesis; vol. 46; 11; (2014); p. 1448 – 1454;,
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Adding a certain compound to certain chemical reactions, such as: 174508-31-7, name is 5,7-Dibromo-2,3-dihydrothieno[3,4-b][1,4]dioxine, 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 174508-31-7, Computed Properties of C6H4Br2O2S

2,5-Bis(thieno[3,2-b]thiophen-2-yl)-2-3,4-ethylenedioxythiophene(TT-EDOT-TT).

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, 5,7-Dibromo-2,3-dihydrothieno[3,4-b][1,4]dioxine, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Xue, Yu; Xue, Zexu; Zhang, Wenwen; Zhang, Wenna; Chen, Shuai; Lin, Kaiwen; Xu, Jingkun; Polymer; vol. 159; (2018); p. 150 – 156;,
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Electric Literature of 327-51-5,Some common heterocyclic compound, 327-51-5, name is 1,4-Dibromo-2,5-difluorobenzene, molecular formula is C6H2Br2F2, 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.

Under an argon atmosphere, to a solution of 1,4-dibromo-2,5-difluorobenzene (1) (20.00 g, 73.6mmol) in diethyl ether (160 mL) was added dropwise 1.6 M n-butyl lithium solution in hexane(1.05 eq, 49 mL) at -78 C, and the mixture was stirred at same temperature for 2 min. Themixture was added quickly to the mixture of dry ice (about 100 g) and diethyl ether (200 mL),and the mixture was warmed up to room temperature. The precipitate was collected by filtration, and washed with diethyl ether. The obtained solid was treated with water (50 mL) and 1 M hydrochloric acid (150 mL), and extracted with diethyl ether. The organic layer was washed with brine and dried. The desiccant was removed by filtration and the filtrate was evaporated in vacuo. The resulting residue was washed with hexane, dried in vacuo to obtain 4-bromo-2,5-difluorobenzoic acid ( 14.8 g, 85 percent) as a pale yellow solid: 1H NMR (DMSO-d6) delta 7.78(1H, dd, J = 6.4, 8.3 Hz), 7.89 (1H, dd, J = 5.9, 9.8 Hz).

The synthetic route of 327-51-5 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Wood, Martyn; Ates, Ali; Andre, Veronique Marie; Michel, Anne; Barnaby, Robert; Gillard, Michel; Molecular Pharmacology; vol. 89; 2; (2016); p. 303 – 312;,
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Reference of 327-75-3, A common heterocyclic compound, 327-75-3, name is 1-Bromo-2,4-bis(trifluoromethyl)benzene, molecular formula is C8H3BrF6, 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.

Intermediate 33. 2-(2,4-Bis-trifluoromethyl-phenoxy)-ethylamine. [00136] Step A:; (2-Hydroxy-ethyl) -carbamic acid tert-butyl ester (0.2 mL, 1.29 mmol) is dissolved in 3 mL dry dimethyl-acetamide. 2-Potassium-1,1,1,3,3,3-hexamethyl- disilazane (0.52 g, 2.6 mmol, 2 equiv. ) is added, followed by 1-bromo-2,4-bis- trifluoromethyl-benzene 31 (0.26 mL, 1.5 mmol, 1.2 equiv. ). The mixture is stirred at 60C under nitrogen for 18 hours. The mixture is cooled, diluted with 50 mL water and extracted with dichloromethane (3 x 50 mL). The combined organic extracts are washed with water and 10% aqueous citric acid, dried over Na2S04 and concentration. Silica gel chromatography (5% to 25% ethyl acetate in hexanes) yielded [2-(2,4-Bis-trifluoromethyl- phenoxy) -ethyl]-carbamic acid tert-butyl ester 32 as a colorless, mobile oil: ‘H-NMR (400 MHz, CDC13) 8 = 7.61 (s, 1H), 7.00 (d, J = 8 Hz, 1H), 6.76 (d, J = 8 Hz, 1H), 5.10 (s, 1H), 4.26 (t, J = 4 Hz, 2H), 3.65 (m, 2H), 1.45 (s, 9H). 19F-NMR (376 MHz, CDC13) 8 =-61.5, – 62.0. No molecular ion could be obtained; a loss of tert-butyl group is observed: MS calculated for C11H10F6NO3 (M+H+-C4H8) 318.1, found 318.3.

The synthetic route of 327-75-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; IRM LLC; WO2005/113519; (2005); A1;,
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Related Products of 68322-84-9, These common heterocyclic compound, 68322-84-9, name is 2-Bromo-1-fluoro-4-(trifluoromethyl)benzene, 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.

j003201 A flask was charged with t-butyl 4-aminopiperidine-1-carboxylate (416 mg, 2.06 mmol, 2.00 equiv), 2-bromo-1-fluoro-4-(trifluoromethyl)benzene (250 mg, 1.03 mmol, 1.00 equiv), DIPEA (403 mg, 3.09 mmol, 3.00 equiv), and dimethyl sulfoxide (10 mL), as described in Example 1, Step 5. The residue was chromatographed on a silica gel column to provide 420 mg (96% yield) of t-butyl 4-((2-bromo-4-(trifluoromethyl)phenyl)amino)piperidine- 1 -carb oxylate as a yell ow oil. LCMS (ESI, m/z): 423 [M+H].

The synthetic route of 68322-84-9 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; ABIDE THERAPEUTICS, INC.; GRICE, Cheryl A.; WEBER, Olivia D.; BUZARD, Daniel J.; SHAGHAFI, Michael B.; WIENER, John J. M.; CISAR, Justin S.; DUNCAN, Katharine K.; (324 pag.)WO2018/217809; (2018); A1;,
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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. 626-40-4, name is 3,5-Dibromoaniline, This compound has unique chemical properties. The synthetic route is as follows., Formula: C6H5Br2N

A solution of 3 (0.7 g, 3.83 mmol) in MeOH (10 mL) was treated with 7 (1.0 g, 4 mmol), refluxed for 12 h, and cooled to roomtemperature to afford 8 (1.6 g, 97%), white crystals, mp 169-170C (MeOH), []D20 -66.72 (c 0.069, DMSO). IR spectrum(, cm-1): 3367-3073 (), 1574 (Ar), 1518 (NH), 1176, 1073 (–), 892 (-, -anomer), 668 (-Br). C12H15Br2NO5.1 NMR spectrum (400 MHz, CDCl3, , ppm, J/Hz): 3.1 (2H, m, -3, 5), 3.17 (3, d, J = 5.2, a), 3.24 (2H, m, -2, 4),3.40-3.65 (1H, ddd, J = 11.8, 5.8, 1.9, H-1), 4.18 (1H, q, J = 5.2, aOH), 4.36 (1H, t, J = 8, H-6), 4.52 (1H, t, J = 5.8, 1-OH),4.96, 4.97 (2H, dd, J = 5.3, 5.5, 3, 5-OH), 5.05 (1H, d, J = 4.8, 4-OH), 6.86 (2H, d, J = 7.6, H-8, 12), 6.89 (1H, d, J = 7.8, NH),6.95 (1H, t, J = 1.6, -10). 13C NMR spectrum (100 MHz, CDCl3, , ppm): 49.1 (a), 61.3 (t, -1), 70.7 (d, -3), 73.5 (d,-5), 77.8 (d, -4), 77.9 (d, -2), 84.5 (d, -6), 115.1 (d, -8, d, -12), 121.5 (d, -10), 123.1 (s, -9, s, -11), 150.7 (s, -7).

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 626-40-4.

Reference:
Article; Makaev; Pogrebnoi; Chemistry of Natural Compounds; vol. 52; 1; (2016); p. 86 – 89; Khim. Prir. Soedin.; (2015); p. 80 – 83,4;,
Bromide – Wikipedia,
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Electric Literature of 49764-63-8, A common heterocyclic compound, 49764-63-8, name is 4,5-Dibromobenzene-1,2-diamine, molecular formula is C6H6Br2N2, 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.

A mixture of 100 ml of toluene, 10 g (0.036 mol) of the compound of example 12.3, 9.65 g (0.079 mol) of phenylboronic acid, 10 g of potassium carbonate and 1 .05 g of tetrakistriphenylphosphinepalladium was heated at 70C for 5 h. Then, the reaction mixture was mixed with water. The phases were separated to give 10.7 g of a crude product which was purified by column chromatography (toluene) to give 8.1 g (79%)

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:
Patent; BASF SE; Koeneman, Martin; Materan, Gabriele; Bagain, Plast Gerhard; Ivanovic, Sorin; St., Robert; (100 pag.)KR2016/38052; (2016); A;,
Bromide – Wikipedia,
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Reference of 327-51-5, 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. 327-51-5, name is 1,4-Dibromo-2,5-difluorobenzene, This compound has unique chemical properties. The synthetic route is as follows.

Under argon stream, 1,2-dimethylimidazole (385 mg, 4.0 mmol), 1,4-dibromo-2,5-difluorobenzene (272 mg, 1.0 mmol)Potassium acetate (393 mg, 4.0 mmol) and palladium acetate (11 mg, 0.05 mmol) were suspended in dimethylacetamide (DMAc, 5.0 mL) and stirred at 150 C. for 48 hours. After allowing to cool, water was added to the reaction mixture, the precipitated solid was collected by filtration,Washing with water yielded the desired 1,4-bis(1,2-dimethylimidazol-5-yl)-2,5-difluorobenzene as a milky white solid (198 mg, 66%).

The chemical industry reduces the impact on the environment during synthesis 1,4-Dibromo-2,5-difluorobenzene. I believe this compound will play a more active role in future production and life.

Reference:
Patent; Tosoh Corporation; Sagami Chemical Research Institute; Aihara, Hidenori; Yamagata, Takuya; Hachiya, Hitoshi; Watanabe, Makoto; Fukuda, Takashi; Ueda, Saori; Miyashita, Masato; (64 pag.)JP2018/168149; (2018); A;,
Bromide – Wikipedia,
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