Month: September 2021

Related Products of 627871-16-3, 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 627871-16-3 as follows.

A mixture of 5-bromo-4-fluoro-2-methylaniline (2.04 g, 10.0 mmol), CuCN (889 mg, 10.0 mmol) and CuI (1.9 g, 10.0 mmol) in NMP was purged with N2 for 5 minutes and then sealed and heated at 195 C. for 30 minutes under microwave condition. The mixture was subjected to standard aqueous workup to give a residue which was purified by silica chromatography to yield 5-amino-2-fluoro-4-methylbenzonitrile (51) (540 mg, 36% yield). MS m/z 151.0 (M+1)+.

According to the analysis of related databases, 627871-16-3, the application of this compound in the production field has become more and more popular.

Reference:
Patent; IRM LLC; YEH, Vince; LI, Xiaolin; LIU, Xiaodong; LOREN, Jon; MOLTENI, Valentina; NABAKKA, Juliet; NGUYEN, Bao; PETRASSI, Hank Michael James; US2013/59846; (2013); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Adding a certain compound to certain chemical reactions, such as: 72678-19-4, name is 2,6-Dibromo-4-(trifluoromethyl)aniline, 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 72678-19-4, Application In Synthesis of 2,6-Dibromo-4-(trifluoromethyl)aniline

EXAMPLE 4 Synthesis of 2-Amino-4,5-dimethyl-1-(2,6-dibromo-4-trifluoromethylphenyl)pyrrole-3-carbonitrile In 15 ml of toluene, 5.5 g of 4-amino-3,5-dibromobenzotrifluoride, 1.9 g of acetoin, and 34 mg of p-toluenesulfonic acid were dissolved. The reaction solution was heated under reflux for 2.5 hours while conducting azeotropic dehydration. To the reaction mixture, 1.42 g of malononitrile was added. The reaction mixture was heated for 4 hours while being concentrated at 180 C. Water was added to the reaction mixture. The reaction mixture was extracted with chloroform, and subsequently, the extract was dried over anhydrous sodium sulfate. After the desiccant was filtered off, the filtrate was concentrated under reduced pressure. The residue was purified by silica gel column chromatography (eluent:hexane-ethyl acetate=5:1), and was allowed to stand for crystallization to yield 1.2 g of 2-amino-4,5-dimethyl-l-(2,6-dibromo-4-trifluoromethylphenyl)pyrrole-3-carbonitrile. m.p. 158-161 C.

If you are interested in these compounds, you can also browse my other articles.Thank you for taking the time to read this article. I hope you enjoyed it.

Reference:
Patent; Taisho Pharmaceutical Co., Ltd.; US6600038; (2003); B1;,
Bromide – Wikipedia,
bromide – Wiktionary

Reference of 112734-22-2, The chemical industry reduces the impact on the environment during synthesis 112734-22-2, name is (4-Bromo-2-fluorophenyl)methanamine, I believe this compound will play a more active role in future production and life.

Preparation of 3-[(4-bromo-2-fluorobenzyl)amino]-1-propanesulfonic acid 4-Bromo-2-fluorobenzylamine hydrochloride (5.0 g, 20.8 mmol) was treated with a saturated solution of K2CO3 (80 mL) and EtOAc (3*80 mL) was added. The organic extracts were combined, dried with Na2SO4, filtered, evaporated under reduced pressure and dried in vacuo. To a solution of 4-Bromo-2-fluorobenzylamine (20.8 mmol) in 50% Pinacolone/Toluene (25 mL) was added 1,3-propane sultone solution (2.3 g, 18.9 mmol). The solution was stirred at reflux for 4 hours. The reaction mixture was cooled to room temperature. The solid material was collected by filtration and washed with acetone (2*20 mL). The solid was suspended in EtOH (40 mL). The suspension was stirred at reflux for 1 hour. The mixture was cooled to room temperature, the solid material was collected by filtration, washed with acetone (2*20 mL) and dried in a vacuum oven (50 C.), affording the title compound, 4.42 g (65%). 1H NMR (D2O, 500 MHz) delta ppm 7.35 (m, 2H), 7.26 (t, 2H, J=7.8 Hz), 4.16 (m, 2H), 3.11 (t, 2H, J=7.8 Hz), 2.85 (t, 2H, J=7.6 Hz), 2.00 (m, 2H). 13C (D2O, 125 MHz) delta ppm 161.98, 159.97, 133.37, 128.50, 124.39, 124.31, 119.79, 119.60, 117.32, 117.19, 48.00, 46.15, 44.40, 21.34. 19F (D2O, 282 MHz) delta ppm -114.64. ES-MS 325 (M-1).

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, (4-Bromo-2-fluorophenyl)methanamine, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Kong, Xianqi; Wu, Xinfu; Bouzide, Abderrahim; Valade, Isabelle; Migneault, David; Bellini, Francesco; US2006/183800; (2006); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Related Products of 630-17-1, 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 630-17-1 as follows.

Example 21; 2-tert-Butyl-l-[(4,4-difluorocycIohexyl)methyl]-5-{[4-(2,2-dimethyIpropoxy)piperidin- l-yl]carbonyl}-lH-benzimidazole; To a solution of NaH (0.017 g, 0.414 mmol) in 2 mL of DMF at 0C under nitrogen, a DMF solution (2 mL) of l-({2-ter/-butyl-l-[(4,4-difluorocyclohexyl)methyl]-lH-benzimidazol-5- yl}carbonyl)piperidin-4-ol (for preparation, see Example 16, Step B) (0.060 g, 0.138 mmol) was added dropwise. The solution was stirred at O0C under nitrogen for 30 min. 1-Bromo- 2,2-dimethylpropane (0.035 mL, 0.276 mmol) was added dropwise and the solution was stirred at 1000C overnight. The reaction was quenched at 00C by addition of aqueous saturated NaHCOs solution and the solvent was concentrated. The residue was dissolved in EtOAc and washed with saturated aqueous NaHCC>3 solution, brine and dried over anhydrous Na2SO4. The product was purified by reversed-phase HPLC using 20-50% CH3CN/H2O and lyophilized to afford the title compound as the corresponding TFA salt. Yield: 45 mg (53%); 1H NMR (400 MHz, METHANOL-D4) delta 0.89 – 0.93 (m, 9 H), 1.51 – 1.64 (m, 2 H), 1.65 – 1.70 (m, 10 H), 1.70 – 1.85 (m, 6 H), 1.94 (s, 1 H), 2.01 – 2.12 (m, 2 H), 2.20 – 2.32 (m, 1 H), 3.14 (d, /=8.59 Hz, 2 H), 3.32 (s, 1 H), 3.54 – 3.62 (m, 2 H), 3.67 (s, 1 H), 3.93 (s, 1 H), 4.57 (d, /=7.62 Hz, 2 H), 7.62 (dd, /=8.69, 1.46 Hz, 1 H), 7.78 (d, /=0.98 Hz, 1 H), 7.99 (d, /=8.59 Hz, 1 H); MS (ESI) (M+H)+ 504.3.

According to the analysis of related databases, 630-17-1, the application of this compound in the production field has become more and more popular.

Reference:
Patent; ASTRAZENECA AB; WO2007/145563; (2007); 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. 16518-62-0, name is 3-Bromo-N,N-dimethylaniline, A new synthetic method of this compound is introduced below., name: 3-Bromo-N,N-dimethylaniline

Into a 50 mL round-bottomed flask were added Pd(PPh3)2Cl2 (0.17 g, 5 mol percent) and 3-bromo-N,N-dimethylaniline (0.60 g, 3 mmol) under an argon atmosphere. Next, 10 mL of 5-(1,3-dioxolan-2-yl)-2-furanylzinc bromide (0.5 M in THF, 5 mmol) was added via a syringe. The resulting mixture was stirred at rt for 3.0 h. Quenched with saturated NH4Cl solution, then extracted with ethyl acetate (10 mL .x. 3). Washed with saturated Na2S2O3 solution and brine, then dried over anhydrous MgSO4. Purification by column chromatography on silica gel (20percent ethyl acetate/80percent heptane) afforded 3-(5-(1,3-dioxolan-2-yl)furan-2-yl)-N,N-dimethylaniline (1g, 0.71 g) in 92percent isolated yield.

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; Rieke, Reuben D.; Kim, Seung-Hoi; Tetrahedron Letters; vol. 52; 10; (2011); p. 1128 – 1131;,
Bromide – Wikipedia,
bromide – Wiktionary

Reference of 61326-44-1, 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. 61326-44-1, name is 1,1,2,2-Tetrakis(4-bromophenyl)ethene belongs to bromides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

(1) A mixture of 3,4,2 mg of palladium acetate, 200 g of K2CO3 and 44 mg of tricyclohexylphosphine was added to the reaction tube under N2, followed by addition of 10 mL of DMF and 130 g of 4-vinylpyridine, followed by heating under reflux for 48 h Room temperature. The solvent was removed by rotary evaporator, the product was extracted with CHCl3, washed with water, the organic phase was collected, and dried over anhydrous Mg2SO4. The final organic phase was purified by silica gel column chromatography eluting with CHCl3: MeOH = 30: 1 to give the final product 6.

The synthetic route of 1,1,2,2-Tetrakis(4-bromophenyl)ethene has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Northwest University; Cao Liping; Li Yawen; Dong Yunhong; (17 pag.)CN107141250; (2017); A;,
Bromide – Wikipedia,
bromide – Wiktionary

Some common heterocyclic compound, 4101-68-2, name is 1,10-Dibromodecan, molecular formula is C10H20Br2, 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. SDS of cas: 4101-68-2

Tempo 1 (0.01 mol) was added to a three-neck flask containing 100 ml dry benzene that is maintained at nitrogen atmosphere. To the flask, sodium hydride (0.015 mol) was added and kept refluxed for 24 hrs. The flask was cooled in ice bath and added 1,10- dibromodecane (0.02 mol) in one portion. The refluxing was then resumed for another 72 hrs. The contents of the flask was cooled in ice bath and added 25ml water and transferred to a separatory funnel. The red upper benzene layer was separated , dried over anhydrous magnesium sulfate and solvent removed by rotory evaporation to get a red oil. The oil was purified by column chromatography on silica gel 60. The material was added to the column and eluted first with about 150 ml hexane that removed the excess of dibromodecane. The desired bromodecanoyl ether of Tempol was eluted with a mixture of hexane and ether(90:10). The red eluate was collected and was found to be pure on thin layer chromatography plates developed using the same solvent mixture. The yield was 0.008 mol (80%).The bromoether of Tempol 0.008 mol and triphenyl phosphine (0,01 mol) were taken in a flask and added 20ml of n-propanol. The contents of the flask was kept refluxed under nitrogen for 72 hrs. The flask was cooled and the solvent was removed by rotory evaporation. The residue was dissolved in 10 ml dichloromethane and added to 100 ml ether with stirring. The precipitated product was collected by decantation of the solvent. The residual semisolid was then purified on silica gel 60 column eluting first with dichloromethane and the desired product was ehited with a mixture of dichloromethane and methanol (90:10). Homogeneous fractions combined and solvent removed to get a red-brown semisolid with a yield of 65%. Purity was ascertained by LC-MS (mass =573.4) .

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 4101-68-2, its application will become more common.

Reference:
Patent; COLBY PHARMACEUTICAL COMPANY; MEDICAL COLLEGE OF WISCONSIN, INC.; WO2008/109740; (2008); A2;,
Bromide – Wikipedia,
bromide – Wiktionary

Related Products of 138526-69-9, 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. 138526-69-9, name is 1-Bromo-3,4,5-trifluorobenzene belongs to bromides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

After adding iodine (10.0 mg, 40.0 mumol) to a tetrahydrofuran solution (190 ml) of magnesium (5.76 g, 237 mmol), 3,4,5-trifluorobromobenzene (50.0 g, 237 mmol) was added at room temperature Was slowly added dropwise.After stirring at the same temperature for 30 minutes, a tetrahydrofuran solution (160 ml) of iodine (66.1 g, 261 mmol) was added at 0 C., and the mixture was stirred at room temperature for 2 hours.The reaction mixture was poured into ice water, neutralized with concentrated hydrochloric acid, and extracted with hexane. The extract was washed with saturated aqueous sodium thiosulfate solution, dried over anhydrous sodium sulfate, and concentrated under reduced pressure. The concentrate was purified by silica gel column chromatography (eluent: ethyl acetate / n-hexane = 1/10) to give the title compound as a yellow oil (yield 45.0 g, yield 70%).

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:
Patent; Hokko Chemical Industry Co., Ltd.; Suzuki, Jun; Wakabayashi, Jin; Murakami, Hideyuki; Onoue, Shinji; (19 pag.)JP2016/84348; (2016); A;,
Bromide – Wikipedia,
bromide – Wiktionary

Related Products of 502496-36-8, The chemical industry reduces the impact on the environment during synthesis 502496-36-8, name is 3-Bromo-5-fluoro-2-methylaniline, I believe this compound will play a more active role in future production and life.

NaNO? (1.93 g, 28.0 mmol) was added to a solution of 3-bromo-5-fluoro-2-methylaniline (4.40 g, 21.6 mmol) in acetic acid (100 mL) and half-concentrated aqueous HC1 (400 mL) at 0 C. After stirring for 5 min at 0 C, CuCl (3.72 g, 37.5 mmol) was added to the reaction mixture. After stirring for 2 h at 0 C, the reaction mixture was warmed to RT and stirring was continued for additional 3 h. Subsequently, the mixture was extracted with Et?0. The combined organic layers were washed with concentrated aqueous NaHCCL-solution (1 x), dried over Na^SCL, filtered, and concentrated in vacuo (bath temperature max. 30 C, vacuum >150 mbar) to give the title compound.

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-Bromo-5-fluoro-2-methylaniline, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; PHARVARIS B.V.; GIBSON, Christoph; SAUPE, Joern; AMBROSI, Horst-Dieter; HAUSTEDT, Lars Ole; (99 pag.)WO2019/101906; (2019); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Application of 201138-91-2, 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. 201138-91-2, name is 4,6-Dibromodibenzo[b,d]furan, This compound has unique chemical properties. The synthetic route is as follows.

0.1 mol of 4,6-dibromodibenzofuran was dissolved in 320 ml of 1,4-dioxane solvent.Stirring with nitrogen,Add 0.09 mol of [4-(triphenylsilyl)phenyl]boronic acid,0.25 mol of potassium carbonate,0.0001 mol of tetrakis(triphenylphosphine)palladium,Warming up to reflux reaction,After 5 hours, the basic reaction of the raw materials was determined by HPLC.The reaction solution was dried under reduced pressure.The residue was subjected to column chromatography to give Intermediate 1-9-1. (Yield: 63%)

The chemical industry reduces the impact on the environment during synthesis 4,6-Dibromodibenzo[b,d]furan. I believe this compound will play a more active role in future production and life.

Reference:
Patent; Beijing Lv Ren Science And Technology Co., Ltd.; Lv Yao; Jia Xueyi; (19 pag.)CN108424420; (2018); A;,
Bromide – Wikipedia,
bromide – Wiktionary