15-Sep-21 News Introduction of a new synthetic route about 452-74-4

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

Synthetic Route of 452-74-4, 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. 452-74-4, name is 1-Bromo-2-fluoro-4-methylbenzene, This compound has unique chemical properties. The synthetic route is as follows.

A degassed solution of 3-amino-furo[3,2-c]pyridine-2-carboxylic acid ethyl ester (300 mg, 1.46 mmol), 4-bromo-3-fluorotoluene (277 mul, 2.19 mmol), Pd2dba3 (67 mg, 0.073 mmol), Xantphos (84 mg, 0.15 mmol) and potassium phosphate tribasic (620 mg, 2.92 mmol) in toluene (10 ml) was heated at reflux under an argon atmosphere for 16 hours. The reaction mixture was concentrated in vacuo and the residue was purified by flash chromatography (Si-SPE, pentane: diethyl ether, gradient 100:0 to 75:25) to afford the title compound as a yellow solid (252 mg, 55%). LCMS (method B): Rx = 3.14 min, M+H+ = 315.

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

Reference:
Patent; GENENTECH, INC.; WO2008/24725; (2008); A1;,
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15-Sep-21 News New downstream synthetic route of 583-70-0

The synthetic route of 583-70-0 has been constantly updated, and we look forward to future research findings.

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. 583-70-0, name is 2,4-Dimethylbromobenzene, A new synthetic method of this compound is introduced below., COA of Formula: C8H9Br

General procedure: A flask furnishedwith a dropping funnel was charged with the aryl/alkylbromide in Et2O. n-BuLi(1.6 M in hexane) diluted with Et2O was added dropwise at -78C. After addition, thereaction was kept at -78C for 10 min and was then allowed to warm to room temperatureand stirred for 30 min. The solution was transferred via cannula to SiCl4 dissolved in Et2Oat 0C. The reaction was stirred for 2 h and was allowed to warm to room temperature. Thesolvent was removed under reduced pressure and the residue dissolved in boiling toluene.Insoluble salts were removed via filtration through cellite and washed with hot toluene. Thesolvent from the resulting clear solution was removed under reduced pressure, followed bypurification via distillation or recrystallization.

The synthetic route of 583-70-0 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Binder, Judith; Fischer, Roland C.; Flock, Michaela; Torvisco, Ana; Uhlig, Frank; Phosphorus, Sulfur and Silicon and the Related Elements; vol. 190; 11; (2015); p. 1980 – 1994;,
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15-Sep News Introduction of a new synthetic route about 4101-68-2

The synthetic route of 4101-68-2 has been constantly updated, and we look forward to future research findings.

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. 4101-68-2, name is 1,10-Dibromodecan, A new synthetic method of this compound is introduced below., Quality Control of 1,10-Dibromodecan

Tempol (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 25 ml 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 synthetic route of 4101-68-2 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; COLBY PHARMACEUTICAL COMPANY; MEDICAL COLLEGE OF WISCONSIN, INC.; US2011/59922; (2011); A1;,
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14-Sep-2021 News Continuously updated synthesis method about 54879-20-8

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

Electric Literature of 54879-20-8, 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. 54879-20-8, name is 2-Bromo-3-methylaniline belongs to bromides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

To a solution of 2-bromo-3-methylaniline (1.0 eq.) in tetrahydrofuran (0.2 M) at 0° C. under N2 atmosphere was added dropwise 1M NaHMDS (2.5 eq.). The reaction was stirred for 15 minutes at 0° C., and a solution of di-tert-butyl dicarbonate in tetrahydrofuran was added. The reaction was warmed to room temperature overnight. The solvent was evaporated, and the resulting residue was quenched with 0.1N HCl aqueous solution. The aqueous suspension was extracted twice with ethyl acetate. The combined organic layers were washed with brine, dried over anhydrous MgSO4, and concentrated en vacuo. The crude material was purified by flash chromatography on a COMBIFLASH® system (ISCO) using 0-5percent ethyl acetate in hexane to give product as light yellow oil.

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

Reference:
Patent; GlaxoSmithKline Biologicals SA; Skibinski, David; Jain, Siddhartha; Singh, Manmohan; O’Hagan, Derek; (124 pag.)US9408907; (2016); B2;,
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14-Sep-2021 News Share a compound : 13633-25-5

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 13633-25-5.

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. 13633-25-5, name is 1-Bromo-4-phenylbutane, This compound has unique chemical properties. The synthetic route is as follows., Quality Control of 1-Bromo-4-phenylbutane

To a stirred solution of tert-Butylprop-2-yn-1-ylcarbamate (300 mg, 1.93 mmol, 1 eq.) in dry DMF (1.93 mL) under nitrogen at 0C, was added NaH (93 mg, 60% in oil, 2.32 mmol, 1.2 eq.) in small portions. After stirring for 15min, (4-bromobutyl)benzene (410 muL, 2.34 mmol, 1.2 eq.) was added dropwise followed by KI(32 mg, 0.19 mmol, 0.1 eq.) and the reaction was warmed up to room temperature for 15 h.After completion of the reaction, water and brine were added and the aqueous layer wasextracted with Et2O (three times). Then, the combined organic layers were dried over MgSO4,filtered and concentrated under vacuum. The crude residue was purified by flash columnchromatography on silica gel (cyclohexane/DCM: 50/50) to afford 1h (446 mg, 1.54 mmol, 80%)as a colorless oil. 1H NMR (300 MHz, CDCl3): delta 7.31-7.24 (m, 2H), 7.21-7.14 (m, 3H), 4.01 (br. s,2H), 3.33 (t, J = 6.6 Hz, 2H), 2.64 (t, J = 7.1 Hz, 2H), 2.16 (t, J = 2.4 Hz, 1H), 1.67-1.56 (m, 4H),1.45 (s, 9H); 13C NMR (100 MHz, CDCl3): delta 155.2 (br. s), 142.4 (br. s), 128.5 (2C), 128.4 (2C),125.8, 80.2, 80.0 (br. s), 71.4 (br. s), 46.4, 36.4 and 36.0 (br. S, rot.), 35.6, 28.6 (br. s), 28.5 (3C),27.6 (br. 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 13633-25-5.

Reference:
Article; Guissart, Celine; Dolbois, Aymeric; Tresse, Cedric; Saint-Auret, Sarah; Evano, Gwilherm; Blanchard, Nicolas; Synlett; vol. 27; 18; (2016); p. 2575 – 2580;,
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14-Sep-2021 News Extended knowledge of 138526-69-9

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.

Synthetic Route of 138526-69-9, A common heterocyclic compound, 138526-69-9, name is 1-Bromo-3,4,5-trifluorobenzene, molecular formula is C6H2BrF3, 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.

General procedure: A mixture of the styrene (3 mmol), the halogenated benzene (3 mmol), triethanolamine (3 mmol) and Pd (II) acetate (0.03 g) was stirred under argon at 100 C for 24 h. The reaction was cooled to 25 C, quenched by the addition of dil. aq. hydrochloric acid (2 N, 10 ml), and extracted with ether (3 × 100 ml). The organic phases were dried (Na2SO4), the solvents evaporated, and the crude product was subjected to chromatography (silica gel, hexane/ethyl acetate mixtures).

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; Csuk, Rene; Albert, Sabrina; Siewert, Bianka; Schwarz, Stefan; European Journal of Medicinal Chemistry; vol. 54; (2012); p. 669 – 678;,
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14-Sep-21 News New learning discoveries about 4333-56-6

The synthetic route of 4333-56-6 has been constantly updated, and we look forward to future research findings.

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. 4333-56-6, name is Bromocyclopropane, A new synthetic method of this compound is introduced below., HPLC of Formula: C3H5Br

[000459j A mixture of Compound 19A (2.0 g, 10 mmol), bromocyclopropane (2.4 g, 20 mmol), Cs2CO3 (9.8 g, 30 mmol) in DMSO (40 mL) was stirred at 170 C for 2 days under high pressure. The mixture was cooled to room temperature and filtered through celite. The filtrate was diluted with ethyl acetate (100 mL), washed with brine (100 mL x 2), dried over sodium sulfate, and concentrated. The crude was purified with column chromatography on silica gel (petroleum ether, 100% v/v) to render Compound 19B. LC-MS (mlz): 247 [M+1] ?H-NMR (CDC13, 400 MHz) major characteristic peaks: 5 (ppm) 0.78-0.82 (m, 4H), 3.7 1-3.73 (m, 1H), 6.95-6.95 (m, 1H), 7.13-7.18 (m, 1H), 7.34-7.36 (m, 1H).

The synthetic route of 4333-56-6 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; BIOMARIN PHARMACEUTICAL INC.; WANG, Bing; WO2015/65937; (2015); A1;,
Bromide – Wikipedia,
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14-Sep-21 News Share a compound : 699-03-6

The chemical industry reduces the impact on the environment during synthesis 699-03-6. I believe this compound will play a more active role in future production and life.

The chemical industry reduces the impact on the environment during synthesis 699-03-6, name is 1-(4-Bromophenyl)-N-methylmethanamine, I believe this compound will play a more active role in future production and life. 699-03-6

The prepared Formula-G was then dissolved in dichloromethane (1.8 L). Triethylamine (1.6 moles, 223.2 mL) was added at 5 C. A solution of methyl chloroformate (1.3 moles, 100.4 mL in dichloromethane (0.2 L) was slowly added, maintaining the temperature of the mixture between about 10 C and 14 C. The reaction solution was stirred at room temperature for 12 hours. Water was added to the reaction mass and the organic phase was separated and concentrated to afford a compound of Formula-E (wherein L=Br, P=methyl carbamate).

The chemical industry reduces the impact on the environment during synthesis 699-03-6. I believe this compound will play a more active role in future production and life.

Reference:
Patent; MYLAN LABORATORIES LTD; JAYACHANDRA, Sureshbabu; SETHI, Madhuresh; KAUSHIK, Vipin Kumar; RAVI, Vijaya, Krishna; TELAGAMSETTY, Bhaskar Kumar; (44 pag.)WO2019/130229; (2019); A1;,
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14-Sep-21 News New learning discoveries about 185122-74-1

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 185122-74-1, its application will become more common.

Some common heterocyclic compound, 185122-74-1, name is 5-Bromo-2,3-dihydro-1H-inden-1-amine, molecular formula is C9H10BrN, 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 5-Bromo-2,3-dihydro-1H-inden-1-amine

To a suspension of 5-bromo-2,3 -dihydro- lH-inden-1 -amine (2.2 g, 10.4 mmol) and NaHC03 (2.6 g, 31.2 mmol) in MeCN (100 mL) was added Boc20 (3.4 mL, 15.6 mmol) at 0 C. The reaction was stirred at rt overnight, then concentrated in vacuo. The residue was dissolved in EtOAc (100 mL). The resulted solution was washed with H20 (50 mL x 2), dried over anhydrous a2S04, filtered and concentrated in vacuo. The residue was purified by a silica gel column chromatography (PE/EtOAc (v/v) =20/1) to give the title compound as a white solid (3.3 g, 100%). MS (ESI, pos. ion) m/z: 257 [M + H – 56]+; NMR (400 MHz, i/6-DMSO) delta (ppm): 1.48 (s, 9H), 1.72-1.85 (m, 1H), 2.49-2.62 (m, 1H), 2.77-2.88 (m, 1H), 2.89-2.98 (m, 1H), 4.67-4.77 (br, 1H), 5.07-5.17 (m, 1H), 7.18 (d, J= 8.0 Hz, 1H), 7.32 (d, J= 8.0 Hz, 1H), 7.36 (s, 1H).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 185122-74-1, its application will become more common.

Reference:
Patent; CALITOR SCIENCES, LLC; SUNSHINE LAKE PHARMA CO., LTD; XI, Ning; WANG, Ruyong; WANG, Liang; WO2014/89324; (2014); A1;,
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9/14/2021 News Continuously updated synthesis method about 608-30-0

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 2,6-Dibromoaniline, its application will become more common.

Related Products of 608-30-0,Some common heterocyclic compound, 608-30-0, name is 2,6-Dibromoaniline, molecular formula is C6H5Br2N, 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.

Example 1 Synthesis of 2,6-dibromobenzenesulfonyl chloride A solution of 2,6-dibromoaniline (10 g, 39.8 mmol) in trifluoroacetic acid (60 mL) and conc. HCl (12 mL) was cooled to 0 C. in an ice bath and treated dropwise with a solution of sodium nitrate (3.4 g, 39.8 mmol) in water (3 mL) over a period of 60 min. To the resulting mixture was added a suspension of copper(I) chloride (2.6 g) and copper(II) chloride (2.6 g) in sulfurous acid (70 mL) and acetic acid (70 mL) over a period of 90 min. After the addition was complete the resulting mixture was stirred at ambient temperature for 45 min. The resulting white precipitate was collected by filtration and dried under the reduced pressure to afford 2,6-dibromobenzenesulfonyl chloride as the white powder (5.2 g, 39%).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 2,6-Dibromoaniline, its application will become more common.

Reference:
Patent; Wexler, Ruth R.; Jacobson, Irina C.; US6399644; (2002); B1;,
Bromide – Wikipedia,
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