Tag: M.W=100-200

Related Products of 1647-26-3, These common heterocyclic compound, 1647-26-3, name is 1-Bromo-2-cyclohexylethane, 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.

Amines 6 (1.0 equivalent) were added to solutions of alkyl halides (1.0 equivalents) in DMF (10ml per gram of 6), followed by TEA (1 .1 equivalents) and the mixture microwaved 60 C for 1 h or until complete consumption of starting materials. The reactions were monitored by TLC using either MeOH:CHCl3 or EA:HEX mixtures and PMA staining. Upon completion, the reaction mixtures were diluted with 15% IPA in CHCI3 (10vol), washed with 1 N NaOH (1vol), dried with Na2S04, filtered and the solvents removed in vacuo. The crude products were purified by FC on silica gel using suitable solvent mixtures from MeOH:CHCl3 or EA:HEX depending on TLC conditions. For highly polar compounds, TEA was added in the mobile phase at concentrations anywhere from 0.1 to 1 %. Product purity was determined by HPLC and product identity confirmed by LC-MS (ESI+) and/or 1H NMR. Alternately, a more convenient work-up procedure was developed by diluting reaction mixture with DMF (1 vol) and stirring with AS-900 (OH-) resin (5g of resin per gram of 6) for 1 h, filtered and the solvents removed in vacuo to give crude product which is purified further.

The synthetic route of 1647-26-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; UNILEVER PLC; UNILEVER N.V.; CONOPCO, INC., D/B/A UNILEVER; ROSA, Jose, Guillermo; LEE, Jianming; MARRERO, Diana; ADAMUS, Jean, Elizabeth; VILLA-MORA, Stella; (51 pag.)WO2016/173817; (2016); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Application of 7073-94-1, 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. 7073-94-1, name is 1-Bromo-2-isopropylbenzene belongs to bromides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

General procedure: Under a nitrogen stream 2- (7-bromotriphenylen-2-yl) -4,4,5,5-tetramethyl-1,3,2-dioxaborolane 5.0 g (11.54 mmol) And 1.78 g (12.70 mmol) of 1-bromo-2- (methylsulfinyl) benzene Was dissolved in 75 ml of toluene, 2M K 2 CO 3 (8 ml) was added thereto, the gas was removed, and 0.73 g of Pd (PPh 3) 4 (5 mol%) was added thereto, followed by stirring at 90 C. for 24 hours. After cooling to room temperature, extracted with dichloromethane, water was removed with MgSO4 and separated into columns using EA / Hexane (1: 3) 2-bromo-7- (2- (methylsulfinyl) phenyl) triphenylene 3.49 g (yield 68%) were obtained.

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-isopropylbenzene, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Doosan Co., Ltd; Bae Hyeong-chan; Kim Seong-mu; Son Hyo-seok; Kim Tae-hyeong; Ra Jong-gyu; (31 pag.)KR101548076; (2015); B1;,
Bromide – Wikipedia,
bromide – Wiktionary

Reference of 1647-23-0, These common heterocyclic compound, 1647-23-0, name is 1-Bromo-3,3-dimethylbutane, 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.

Example 218 (R)-2-Ethyl-piperazine-1-carboxylic acid 3-(3,3-dimethyl-butoxy)-2,6-difluoro-benzyl ester hydrochloride According to example 207 the title compound was synthesised from (R)-2-Ethyl-piperazine-1,4-dicarboxylic acid 4-tert-butyl ester 1-(2,6-difluoro-3-hydroxy-benzyl)ester and 3,3-dimethylbutyl bromide. MS (ISP): 385 (M+H)+.

The synthetic route of 1647-23-0 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Adams, David Reginald; Bentley, Jonathan Mark; Davidson, James Edward Paul; Dawson, Claire Elizabeth; George, Ashley Roger; Mansell, Howard Langham; Mattei, Patrizio; Mizrahi, Jacques; Nettekoven, Matthias Heinrich; Pratt, Robert Mark; Roever, Stephan; Roffey, Jonathan Richard Anthony; Specklin, Jean-Luc; Stalder, Henri; Wilkinson, Kerry; US2002/143020; (2002); A1;,
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. 134168-97-1, name is 3-Bromo-5-fluoroaniline belongs to bromides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. category: bromides-buliding-blocks

1000mL 4 neckround bottom flask was charged with 3-bromo-5-fluoroaniline 30.5 g (0.16 mole) and Pd (PPh3) 47.4 g (0.006mole) of potassium carbonate and 88.1 g (0.64 mole) and 3-pyridineboronic acid 23.4 put g (0.19 mole), toluene was put into210 mL, 160 mL ethanol, 90 mL of water was refluxed for 12 hours. To complete the reaction, and the organic layer wasseparated and the water layer was extracted twice with 100 mL toluene. Formed organic layer was concentrated underreduced pressure and recrystallized with methanol to intermediate 6a(21.1 g, 70.0%) was obtained.

The synthetic route of 134168-97-1 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; SFC CO., LTD.; KIM, JEONG SOO; RYU, YEON KWON; KO, SANG WON; LEE, SU JIN; KIM, JI HWAN; PARK, JIN JOO; (44 pag.)KR2015/129486; (2015); A;,
Bromide – Wikipedia,
bromide – Wiktionary

Electric Literature of 1647-23-0, 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. 1647-23-0, name is 1-Bromo-3,3-dimethylbutane belongs to bromides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

The title compound was prepared from 50 mg 3-ter/-butylquinolin-2(lH)-one (Preparative Example 1, Step E), 55 mg l-bromo-3,3-dimethylbutane, and 143 mg cesium carbonate in 1 mL DMF at 55C for 12 hours. It was separated from less polar side-product 3-ter*-butyl-2-(3,3-dimethylbutoxy)-7- methoxyquinoline using RP-etaPLC. The isomers were identified by comparison of NMR with isomers in Preparative Example 1, Step F. 1H NMR in CDCl3 at 500 MHz: 7.53 (s, IH), 7.46 (d, 9.0 Hz5 IH), 6.81 (dd, 9.0 & 2.0 Hz, IH), 6.77 (d, 2.0 Hz, IH), 4.29 (m, 2H), 3.92 (s, 3H), 1,68 (m, 2H)5 1.44 (s, 9H), 1.26 (s, 9H).

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-3,3-dimethylbutane, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; MERCK & CO., INC.; WO2007/108968; (2007); A2;,
Bromide – Wikipedia,
bromide – Wiktionary

Adding a certain compound to certain chemical reactions, such as: 1073-39-8, name is 3-Bromobicyclo[4.2.0]octa-1,3,5-triene, 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 1073-39-8, Quality Control of 3-Bromobicyclo[4.2.0]octa-1,3,5-triene

To a mixture of 3-bromobicyclo[4.2.0]octa-1 (6),2,4-triene (300 mg, 1.64 mmol, 1.10 equiv) in THF (4 mL) was added n-BuLi (2.5 M in hexane, 0.66 mL, 1.64 mmol, 1.00 equiv) dropwise at -78C. The reaction mixture was stirred for 30 min at -78C. To the resulting mixture was then added a solution of 4- (benzyloxy)-5-bromo-2-(dimethylamino)benzaldehyde (500 mg, 1.50 mmol, 1.00 equiv) in THF (1 mL) dropwise at -78 C. The reaction mixture was stirred for 3 h at -78C. NH4CI/H2O was added and the mixture was extracted with EtOAc thrice. The combined extracts were washed with brine and dried over Na2S04, then concentrated and purified by chromatography on silica gel (3: 1 PE/EA) to yield (4-(benzyloxy)-5-bromo-2-(dimethylamino)phenyl)(1,2- dihydrocyclobutabenzen-4-yl)methanol as a colorless oil.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 3-Bromobicyclo[4.2.0]octa-1,3,5-triene, and friends who are interested can also refer to it.

Reference:
Patent; JANSSEN PHARMACEUTICA NV; GAUL, Micheal; KUO, Gee-Hong; XU, Guozhang; LIANG, Yin; (218 pag.)WO2018/89449; (2018); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Reference of 18087-73-5, A common heterocyclic compound, 18087-73-5, name is 3-Bromoimidazo[1,2-b]pyridazine, molecular formula is C6H4BrN3, 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.

EXAMPLE 28; N-[ (1R,6S)-6-Amino-2,2-difluorocyclohexyl]-5-chloro-4-(imidazo[1,2-b]pyridazin-3-yl)-1,3- thiazole-2-carboxamide; Step 1. 1 -(Imidazo[1,2-b]pyridazin-3-yl)ethanone; 3-Bromoimidazo[1,2-b]pyridazine (1.0 g, 5.05 mmol), tributyl(l-ethoxyvinyl)tin (3.41 mL, 10.1 mmol), and PdCb(PPh3)2 (354 mg, 0.505 mmol), were added to a sealed tube. DMF (25.2 mL) was added and the reaction purged with nitrogen for 5 minutes. The reaction was heated at 100 C for 18 h. The reaction was cooled to room temperature and quenched with aqueous saturated sodium bicarbonate. The aqueous layer was extracted with ethyl acetate (x 3) and the combined organic layers were dried with magnesium sulfate, Filtered, and concentrated under reduced pressure. The residue was diluted with methanol (10 mL) and HCl in 1,4-dioxane (1.26 mL, 5.05 mmol, 4M) was added. The solution was stirred at room temperature for 1 h. The reaction was then quenched with aqueous saturated sodium bicarbonate and extracted with ethyl acetate (x 3). The combined organic layers were dried with magnesium sulfate, filtered, and concentrated under reduced pressure. The residue was purified by flash chromatography to afford the title compound. 1H NMR (500 MHz, CD3SOCD3) delta 8.76 (d, 1H); 8.55 (s, 1H); 8.31 (d, 1H); 8.49 (dd, 1H); 2.64 (s, 3H). LRMS (APCI) calc’d for (C8H7N3O) [M+H]+, 162.1; found 162.1.

The synthetic route of 18087-73-5 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; MERCK SHARP &; DOHME CORP.; ALTMAN, Michael, D.; BILODEAU, Mark, T.; LIM, Jongwon; NORTHRUP, Alan; STANTON, Matthew, G.; TAOKA, Brandon, M.; WO2010/83145; (2010); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Related Products of 348-57-2, These common heterocyclic compound, 348-57-2, name is 1-Bromo-2,4-difluorobenzene, 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.

EXAMPLE 17 Preparation of 4-(2,4-difluorophenyl)-anisole from 4-methoxyphenylmagnesiumbromide and palladium acetate/triphenylphosphine (0.05percent) A suspension of magnesium turnings (1.54 g; 63.3 mmoles–Pometon) in tetrahydrofuran (16.02 g) was heated at 65¡ã C. under stirring and under nitrogen. Then, iodine (0.02 g) and, after 30 minutes, 4-bromoanisole (11.69 g; 62.5 mmoles), in 1 hour, were added to the reaction mixture. At the end of the addition, the reaction mixture was kept at 75¡ã C. for 1 hour and, then, decanted obtaining a solution of 4-methoxyphenylmagnesiumbromide (solution A). A mixture of 1-bromo-2,4-difluorobenzene (11.4 g; 59.1 mmoles), palladium acetate (0.00663 g; 0.0295 mmoles–Janssen) and triphenylphosphine (0.03074 g; 0.1172 mmoles–Fluka) was de-aerated by vacuum/nitrogen at 25¡ã C. The mixture was heated at 85¡ã C., kept under stirring for 15 minutes and, then, solution A was added in 3 hours. At the end of the addition, the reaction mixture was kept at 85¡ã C. for 30 minutes. After cooling at 60¡ã C., a solution of 37percent hydrochloric acid (2 ml) in water (10 ml) was added in 20 minutes. The mixture was cooled at 40¡ã C. and the phases were separated. The solvent of the organic phase was evaporated under reduced pressure obtaining the desired compound (92percent yield).

Statistics shows that 1-Bromo-2,4-difluorobenzene is playing an increasingly important role. we look forward to future research findings about 348-57-2.

Reference:
Patent; Zambon Group S.p.A.; US5312975; (1994); A;,
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 7745-91-7 as follows. Product Details of 7745-91-7

(TrifluoromethvDBenzamide (Intermediate 33″)33[0232] To a solution of 3-bromo-4-methylbenzenamine (0.82 g, 4.4 mmol) in anhydrous CH2Cl2 (40 mL) was added 3-(trifluoromethyl)benzoyl chloride (0.72 ml, 4.85 mmol) and triethylamine (2.5 ml, 17.6 mmol). The mixture was stirred overnight at room temperature. The saturated NaHCCb (80 mL) was added and the mixture was stirred for 5 min. The organic layer was separated and aqueous was extracted with CH2CI2 (3 x 20 mL). The combined organic solution was dried (Na2SO4). The solvent was removed in vacuo. The title compound was afforded as a yellow solid (1.48 g, 94%).

According to the analysis of related databases, 7745-91-7, the application of this compound in the production field has become more and more popular.

Reference:
Patent; TARGEGEN, INC.; WO2008/8234; (2008); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Reference of 2695-47-8,Some common heterocyclic compound, 2695-47-8, name is 6-Bromo-1-hexene, molecular formula is C6H11Br, 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.

Step A: Preparation of 2,2,2-trifluoro-N-(hex-5-enyl)-N-methylacetamide 31a. Sodium hydride (60% dispersion in mineral oil, 31.5 g, 1.28 eq.) was slowly added under nitrogen atmosphere to a solution of N-methyl-2,2,2-trifluoroacetamide (100 g, 1.28 eq.) in DMF (500 mL) at 0 C. The reaction mixture was stirred for 90 min at 0 C., and then 6-bromo-1-hexene (100 g, 1 eq.) was added dropwise over 45 min. The reaction mixture was allowed to warm up to room temperature, and stirred for 3 days at room temperature. The reaction mixture was then poured into water and extracted tree time with EtOAc. The combined organics layers were dried over anhydrous sodium sulphate and concentrated under reduced pressure. The residue was purified by flash chromatography on silica gel to produce compound 31a as colorless oil in 56% yield. 1H NMR (DMSO-d6, 400 MHz) delta 1.27-1.38 (m, 2H), 1.48-1.60 (m, 2H), 2.00-2.06 (m, 2H), 2.93-3.07 (2m, 3H), 3.35-3.40 (m, 2H), 4.92-5.04 (m, 2H), 5.73-5.83 (m, 1H).

The synthetic route of 2695-47-8 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Idenix Pharmaceuticals, Inc.; US2009/202480; (2009); A1;,
Bromide – Wikipedia,
bromide – Wiktionary