Tag: M.W=200-300

Related Products of 4549-33-1, These common heterocyclic compound, 4549-33-1, name is 1,9-Dibromononane, 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.

2,2, 12, 12-Tetramethyltridecanedioic acid diethyl ester (153).; Under N2 atmosphere and at-78 C, a solution of lithium diisopropylamide (2 M in heptane/THF/ethylbenzene, 52.5 mL, 105 mmol) was added dropwise to a solution of ethyl isobutyrate (17.4 g, 150 mmol) in THF (50 mL). The mixture was stirred for 1 h and 1, 9-dibromononane (151, 14.3 g, 50 mmol) was added, followed by DMPU (4.4 g, 34.3 mmol). The mixture was stirred for 30 min and the cooling bath was removed. After 30 min, the THF was evaporated under reduced pressure. The residue was diluted with saturated NH4CI ‘bluti6’n” (300 mL) aSd’-exti’Scted with ethyl acetate (3 x l00 mL). The combined organic layers was washed with brine (200 mL), 5 % aqueous HC1 (100 mL) and saturated NaHC03 solution (50 mL), and dried over Na2S04. The solvent was removed under reduced pressure and the residue was distilled in high vacuo to give 153 (14.0 g, 79 %) as an oil. Bp 150-151 C/0. 1 mmHg. 1H NMR (CDC13) : 8 (ppm): 4.08 (q, J= 7. 2, 4 H), 1.48-0. 98 (m, 18 H), 1.21 (t, J= 7.2, 6 H), 1.12 (s, 12 H). 13C NMR (CDCl3) : 5 (ppm) : 178.1, 60.0, 42.1, 40.7, 30.0, 29.4, 25.1, 24. 8, 14.2.

The synthetic route of 4549-33-1 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; ESPERION THERAPEUTICS, INC.; WO2005/68410; (2005); A1;,
Bromide – Wikipedia,
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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. 50548-45-3, name is 1-Bromodibenzo[b,d]furan, This compound has unique chemical properties. The synthetic route is as follows., Recommanded Product: 1-Bromodibenzo[b,d]furan

Into a 1 L four-necked round bottom flask equipped with a stirrer, a Liebig condenser fitted with a calcium chloride tube, a nitrogen inlet tube, a 200 mL isobaric dropping funnel and a thermometer, 34.5 g of the bromide obtained in the above (139.6 mmol) of dehydrated THF and 325 mL of dehydrated THF, and the mixture was cooled to -60 ° C. or lower in an acetone-dry ice bath under a nitrogen stream. Subsequently, 106 mL (167.6 mmol) of n-BuLi was added dropwise at -50 ° C. or lower, then the isobaric dropping funnel was washed with 100 mL of THF and added to the reaction solution. Subsequently, after postreaction at -50 ° C. or lower for 1 hour, 43 mL (181.6 mmol) of [B (i-PrO) 3] was added dropwise at -45 ° C. or lower. Subsequently, the isobaric dropping funnel was washed with 80 mL of THF and added to the reaction solution, followed by stirring at -45 ° C. or lower for 30 minutes. The acetone-dry ice bath was removed, the temperature was returned to room temperature, and the reaction was continued for additional 20 hours to obtain boron To obtain a reaction solution.Next, 24 mL of concentrated hydrochloric acid and 241 mL of water were placed in a 1 L four-necked round bottom flask equipped with a stirring device, a Liebig condenser (not required), a 1 L dropping funnel and a thermometer, ° C. Subsequently, the boron reaction solution was dropped at a temperature not exceeding 10 ° C., and the mixture was stirred at 10 ° C. or less for 1 hour, then returned to room temperature and stirred for 3 hours.The obtained reaction solution was transferred to a 1 L separating funnel, the organic layer was separated, and the aqueous layer was extracted with 340 mL of ethyl acetate. Next, the organic layers were combined and washed with saturated brine 240 mL, dried over magnesium sulfate, magnesium sulfate was removed by suction filtration, and the solvent was distilled off under reduced pressure. Subsequently, 220 mL of n-heptane was added to the obtained crude crystals, rinsed at 50 ° C. for 1 hour, cooled to room temperature and filtered by suction to obtain 21.6 g of the desired boronic acid (yield 72.8percent)

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 50548-45-3.

Reference:
Patent; YAMAGATA UNIVERSITY; CHEMIPRO KASEI KAISHA LIMITED; KIDO, JUNJI; SASABE, HISAHIRO; TAKAHASHI, JUN; NAGAI, NAGAI; (723 pag.)JP2018/90561; (2018); A;,
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. 58971-11-2, name is 3-Bromophenethylamine belongs to bromides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Computed Properties of C8H10BrN

General procedure: Amine (1 equiv.) and aldehyde (5 equiv.) were dissolved in a 1:1 mixture of methanol/phosphatebuffer (10 mL, 0.25 M solution at pH 6). The resulting solution was stirred at 100 C for 12 h. The crudemixture was cooled to r.t. and purified by preparative HPLC (Gradient 1). Fractions containing thedesired product were combined, concentrated under vacuum and co-evaporated with methanol(3 x 20 mL).

The synthetic route of 58971-11-2 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Pesnot, Thomas; Gershater, Markus C.; Edwards, Martin; Ward, John M.; Hailes, Helen C.; Molecules; vol. 22; 4; (2017);,
Bromide – Wikipedia,
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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. 393-37-3, name is 5-Bromo-2-fluorobenzotrifluoride, This compound has unique chemical properties. The synthetic route is as follows., Computed Properties of C7H3BrF4

A mixture of sodium thiomethoxide (0.317g) and 5-bromo-2-fluorobenzotrifluoride (L. OG) in DMF (4ML) was heated at 50C for lh then poured into water and extracted with isohexane. The organics were washed with brine, dried and evaporated under reduced pressure. Yield 0. 762g H NMR DMSO-d6: 8 7.74 (1H, d); 7.59 (1H, dd); 7.22 (1H, d); 2.51 (3H, s)

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 393-37-3.

Reference:
Patent; ASTRAZENECA AB; ASTRAZENECA UK LIMITED; WO2005/18529; (2005); A2;,
Bromide – Wikipedia,
bromide – Wiktionary

Synthetic Route of 61613-22-7, The chemical industry reduces the impact on the environment during synthesis 61613-22-7, name is 2-Bromo-N-phenylaniline, I believe this compound will play a more active role in future production and life.

The 34·7 g (140 mmol) of 2-bromo diphenylamine initially introduced 350ml of absolute THF and cooled to -78 C, and the THF was added to 112 ml (280 mmol) of 2.5 Mu n-BuLi . The mixture was then thawed to -10 C stirred for another 1 h at this temperature. Was slowly added dissolved in 600ml of THF of 30 g (86 mmol) 10-biphenyl-4-yl-2,7-diphenyl-10H- acridine-9-one. The mixture is then stirred for another 24 h at room temperature. 100 ml of a solution of ammonium chloride was added, stirring continued briefly, and the organic phase was separated, and the solvent removed in vacuum. The residue was suspended at 40 C in 750 ml of warm glacial acetic acid, added to 60 ml of concentrated hydrochloric acid to the suspension, and the mixture was then stirred at room temperature for another 8 h. After cooling, it is filtered off with suction the precipitated solid was washed once with 100 ml of water, washed three times with each 100 ml of ethanol and finally recrystallized from heptane. Yield: 35.3 g (54 mmol), 77% theory.

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, 2-Bromo-N-phenylaniline, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; MERCK PATENT GMBH; PFISTER, JOCHEN; VOGES, FRANK; MONTENEGRO, ELVIRA; MUJICA, FERNAUD, TERESA; (101 pag.)TW2016/2091; (2016); A;,
Bromide – Wikipedia,
bromide – Wiktionary

Application of 14659-58-6, 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. 14659-58-6 name is 2-Bromo-5-fluoro-1,3-dimethylbenzene, 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.

In Step 2, Compound 78 (10 g) was converted Compound 79 using methyl 2- mercaptoacetate in piperidine/pyridine at 100 C. The reaction was stirred for 4 hour prior to purification that yielded Compound 79 (11.7 g). In Step 3, Compound 79 (2 g) was converted to benzothiophene Compound 72 using SOCI2 in xylenes/pyridine. The reaction was heated to 120 C and allowed to stir overnight. In Step 4, Compound 72 is subjected to n-butyl lithium and 2- bromo-5-fluoro-1,3-dimethylbenzene to afford Compound 73. In Step 5, Compound 73 is demethylated using BBr3 to afford Compound 74. In Step 6, Compound 74 is reacted with sodium hydride and benzyl bromide to afford Compound 75. In Step 7, Compound 75 is mixed with Compound 38 and cesium carbonate in DMSO to afford Compound 76. In Step 8, the benzyl protecting group of Compound 76 is removed by hydrogenation to afford Compound 112.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 2-Bromo-5-fluoro-1,3-dimethylbenzene, and friends who are interested can also refer to it.

Reference:
Patent; G1 THERAPEUTICS, INC.; STRUM, Jay, Copeland; (187 pag.)WO2020/37251; (2020); 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. 112734-22-2, name is (4-Bromo-2-fluorophenyl)methanamine, A new synthetic method of this compound is introduced below., Quality Control of (4-Bromo-2-fluorophenyl)methanamine

At 0C, p-toluenesulfonyl chloride (4.00g, 21mmol) was added in portion to a solution of 5-bromo-2-fluorobenzlamine (4.08g, 20mmol) and triethylamine (4.04g, 40mmol) in DCM (60mL). The mixture was reacted at 0C for 30mins, followed by removing the ice bath, further reacting at room temperature for 16hrs, then being concentrated under reduced pressure. The residue was purified by silica column chromatography (PE:EA = 5:1) to give compound 9-f (5.30g, yield 74%). LC-MS (ESI): m/z = 358 [M+H]+.

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; Shanghai Yingli Pharmaceutical Co. Ltd.; XU, Zusheng; ZHANG, Nong; SUN, Qingrui; WU, Tianzhi; (104 pag.)EP3275867; (2018); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Related Products of 1435-51-4, These common heterocyclic compound, 1435-51-4, name is 1,3-Dibromo-5-fluorobenzene, 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.

To a mixture of tris(dibenzylideneacetone)dipalladium (0.20 g, 0.22 mmol), 9,9-dimethyl-4,5-bis(diphenylphosphine)xanthene (0.13, 0.22 mmol) and cesium carbonate (5.0 g, 15.41 mmol) under N2 gas was added acetamide (0.90, 14.73 mmol), l,3-dibromo-5- fluorobenzene (2.8 g, 10.83 mmol) and dioxane (22 mL). The reaction mixture was heated at 8O0C overnight and concentrated under reduced pressure. Purification by flash chromatography (silica, 50:50 ethyl acetate/hexane) gave N-(3-bromo-5-fluorophenyl)acetamide (3.51 g, quantitative). Retention time (min) = 1.945, method [4], MS(ESI) 232.0 (M+Eta).

The synthetic route of 1435-51-4 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; ELAN PHARMACEUTICALS, INC.; SHAM, Hing, L.; KONRADI, Andrei, W.; HOM, Roy, K.; PROBST, Gary, D.; BOWERS, Simeon; TRUONG, Anh; NEITZ, R., Jeffrey; SEALY, Jennifer; TOTH, Gergely; WO2010/91310; (2010); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Application 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.

To a solution of l,4-dibromo-2,5-difluorobenzene (12.6 g, 46.3 mmol) in toluene (300 mL) cooled to -78 C was added butyllithium (18.5 mL, 46.3 mmol) at such a rate that the internal temperature did not exceed -50 C and the reaction was stirred for 45 minutes. To the reaction was added N, N-dimethylacetamide (4.84 g, 55.6 mmol). The reaction was stirred at -78 C and then warmed to ambient temperature over a period of 4 hours. The reaction was quenched by adding water (300 mL) followed by the addition of EtOAc (500 mL) and the layers were separated. The organic layer was washed with brine (100 mL), dried over MgS04, filtered and concentrated in vacuo. The crude material was chromatographed eluting with 10% EtOAc/Hexane to give l-(4-bromo-2,5- difluorophenyl)ethanone (5 g, 21.3 mmol, 45.9 % yield).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 1,4-Dibromo-2,5-difluorobenzene, its application will become more common.

Reference:
Patent; ARRAY BIOPHARMA INC.; FELL, Jay Bradford; FISCHER, John P.; HINKLIN, Ronald J.; WO2013/74641; (2013); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

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 62871-09-4 as follows. Formula: C10H19Br

To a stirred solution of (S)-nicotine (0.52 g, 3.2 mmol) in AcOH (10 ml) was added 10-bromo-dec-1-ene (1.66 g, 7.58 mmol).The mixture was heated at reflux for 3 days. AcOH was evaporated and the residue was dissolved in CHCl3.The mixture was washed with saturated aqueous NaHCO3, water and brine successively and dried.Evaporation of the solvent followed by titration with ether afforded 0.74 g (61%) of (S)-1-dec-9-enyl-3-(1-methyl-pyrrolidin-2-yl)-pyridinium bromide (NDNB-9e) as a brown oil. 1H NMR (300 MHz, CDCl3) delta 9.65 (1H, d, J=5.1 Hz), 9.14 (1H, s), 8.41(1H, d, J=8.1 Hz), 8.09 (1H, dd, J=8.1, 5.1 Hz), 5.75 (1H, m), 4.88-5.10 (4H, m), 3.54 (1H, t, J=8.1 Hz), 3.23 (1H, m), 2.45 (2H, m), 2.22 (3H, s), 1.70-2.10 (6H, m), 1.61 (1H, m), 1.10-1.40 (10H, m); 13C NMR (75 MHz, CDCl3) delta 146.46, 144.39, 143.74, 142.97, 139.07, 128.50, 114.33, 67.17, 62.25, 56.92, 40.74, 36.11, 33.93, 32.35, 29.42, 29.24, 29.15, 29.03, 26.35, 23.41.

According to the analysis of related databases, 62871-09-4, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Crooks, Peter A.; Dwoshin, Linda; Xu, Rui; Ayers, Joshua T.; US2003/225142; (2003); A1;,
Bromide – Wikipedia,
bromide – Wiktionary