Month: May 2021

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. 66417-30-9, name is 2-Bromo-1-methyl-4-(trifluoromethyl)benzene, A new synthetic method of this compound is introduced below., Product Details of 66417-30-9

Butyl lithium (1.6 M in hexane, 2.6 mL, 4.18 mmol) was added dropwise to a solution of 2-methyl-5-(trifluoromethyl)bromobenzene (1 g, 4.18 mmol) in Et20 (15 mL) at -78 C. The r.m. was stirred at -78 C for 20 min and then l-(tert-butyldimethylsilyloxy)-2- propanone (0.827 g, 4.39 mmol) in Et20 (5 mL) was added and the r.m. was further stirred for 2 h at -78 C. The r.m. was then quenched with water and the product was extracted with EtOAc. The organic layer was dried over MgS04, filtered and the solvent was removed in vacuo. The crude product was purified by flash column chromatography (silica; heptanes/EtOAc 100/0 to 90/10). The fractions containing the product were collected and concentrated in vacuo to give intermediate 46 (1.036 g, 71%).

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; JANSSEN PHARMACEUTICA NV; BISCHOFF, Francois, Paul; VELTER, Adriana, Ingrid; ROMBOUTS, Frederik, Jan, Rita; DE CLEYN, Michel, Anna, Jozef; VAN BRANDT, Sven, Franciscus, Anna; GIJSEN, Henricus, Jacobus, Maria; ZAVATTARO, Chiara; VAN DEN KEYBUS, Frans, Alfons, Maria; WO2014/111457; (2014); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

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. 43204-63-3, name is Bis(2-Bromoethyl)amine hydrobromide, This compound has unique chemical properties. The synthetic route is as follows., Recommanded Product: Bis(2-Bromoethyl)amine hydrobromide

EXAMPLE 148 8-Aminocarbostyril (15.47 g, 96.6 mmols) and bis(beta-bromoethyl)amine hydrobromide (33 g, 106 mmols) were suspended in DMF and the suspension was stirred at 70 to 80 C. for 10 hours. After adding 5.1 g of sodium carbonate the reaction mixture was stirred at the same temperature as above for 7 hours. After distilling off the solvent under reduced pressure, methanol was added to the residue to crystallize. The crude crystals thus obtained were recrystallized from methanol-ether to give 5.1 g of 8-(1-piperazinyl)carbostyril hydrobromide, m.p. above 300 C., colorless scales.

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 43204-63-3.

Reference:
Patent; Otsuka Pharmaceutical Co., Ltd.; US4415572; (1983); A;,
Bromide – Wikipedia,
bromide – Wiktionary

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. 30432-16-7, name is 1,4-Dibromo-2,3-bis(bromomethyl)but-2-ene, This compound has unique chemical properties. The synthetic route is as follows., HPLC of Formula: C6H8Br4

4-Hydroxy benzonitrile (3) (1.19 g, 10 mmol) and potassium hydroxide (0.56 g, 10 mmol) were dissolved in absolute ethanol. 1,1,2,2-tetrayl-tetramethylene-tetrabromide (1) (1.00 g, 2.5 mmol) was then added into this solution. The reaction mixture was refluxed for 8 h. The solution was cooled and filtrated. The white solid obtained was washed with H2O, alcohol and crystallized from DMF. Yield: 1.14 g (83%). mp 212-214 C. IR (ATR, cm-1): 3080 nu(=CH), 2949 nu(-CH2), 2222 nu(C?N), 1601 nu(C=C), 1573, 1504 nu(C-C), 1298, 1236, 1113 nu(C-O-C), 1086 nu(Ester C-O-C),833 nu(1,4-disubst.), 695 deltar(CH2). 1H NMR (400 MHz, DMSO-d6, delta ppm): 4.94 (s, 8H, O-CH2), 7.08 (d, AA’ , 8H, J = 16.0 Hz, Ar-H), 7.72 (d, AA’ , 8H, J = 16.0 Hz, Ar-H). 13C NMR (100 MHz, DMSOd6, delta ppm): 65.55 (O-CH2), Ar-C: [103.60 (C), 116.26 (CH),134.53 (CH), 162.06 (C)], 135.50 (C=C); 119.52 (C?N). Analysis (% calculated/found) for C34H24N4O4 (Mw 552.58) C: 73.90/73.81;H: 4.38/4.44; N: 10.14/10.17. MS(ESI-m/z): 575.36 [M+Na]+.

According to the analysis of related databases, 30432-16-7, the application of this compound in the production field has become more and more popular.

Reference:
Article; Er, Mustafa; De?irmencio?lu, Ismail; Tahtaci, Hakan; Spectrochimica Acta Part A: Molecular and Biomolecular Spectroscopy; vol. 139; 1; (2015); p. 68 – 74;,
Bromide – Wikipedia,
bromide – Wiktionary

Reference of 112279-72-8,Some common heterocyclic compound, 112279-72-8, name is 4-Bromo-2,3-difluoroaniline, molecular formula is C6H4BrF2N, 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 Compound (G-2) (78 g, 375 mmol) in anhydrous dichloromethane (250 mL) was added acetic anhydride (53.2 ml, 563 mmol) at room temperature, then the reaction mixture was stirred for 1 hour. After the completion of the reaction, the insoluble residue was collected by filtration to give Compound (G-3) (85.3 g, 91%).Compound (G-3);1H-NMR (DMSO-d6) delta: 2.10 (s, 3H), 7.48 (t, J=7.2 Hz, 1H), 7.72 (t, J=7.2 Hz, 1H), 10.32 (s, 1H).

The synthetic route of 112279-72-8 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Shionogi & Co., Ltd.; US2012/253040; (2012); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Synthetic Route of 58534-95-5, These common heterocyclic compound, 58534-95-5, name is 3-Bromo-2-fluoroaniline, 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.

Copper(I) iodide (1.002 g, 5.26 mmol) was added in one portion to 3-bromo-2-fluoroaniline (5 g, 26.31 mmol), N1,N2-dimethylethane-1,2-diamine (0.464 g, 5.26 mmol) and sodium iodide (7.89 g, 52.63 mmol) in 1,4-dioxane (10 mL) at 25 C over a period of 1 minute under nitrogen. The resulting suspension was stirred at 110 C for 1 day. The reaction mixture was filtered through celite and concentrated in vacuo. The crude product was purified by flash silica chromatography using a gradient 5 – 30 % EtOAc in petroleumether as mobile phase. Pure fractions were evaporated in vacuo to afford 2-fluoro-3- iodoaniline (5.00 g, 80 %) as a brown oil.?H NMR (400 MHz, DMSO-d6) 5 5.32 (bs, 2H), 6.59 – 6.83 (m, 2H), 6.83 – 6.93 (m, 1H). m/z (ES+), [M+H] 238.

Statistics shows that 3-Bromo-2-fluoroaniline is playing an increasingly important role. we look forward to future research findings about 58534-95-5.

Reference:
Patent; ASTRAZENECA AB; NILSSON, Karl, Magnus; ASTRAND, Annika, Birgitta, Margareta; BERGGREN, Anna, Ingrid, Kristina; JOHANSSON, Johan, R.; LEPISTOe, Matti, Juhani; KAWATKAR, Sameer, Pralhad; SU, Qibin; KETTLE, Jason, Grant; (143 pag.)WO2018/134213; (2018); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

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.

To a vial were added the product of Example 1H (0.150 g, 0.373 mmol), (2- bromoethyl)cyclohexane (0.142 g, 0.746 mmol), cesium carbonate (0.364 g, 1.12 mmol), and /V,/V-dimethylformamide (1.5 mL). The resulting mixture was stirred at ambient temperature. After 13 hours, the reaction mixture was partitioned between 1 M hydrochloric acid (25 mL) and ethyl acetate (15 mL). The layers were separated and the aqueous phase was extracted with ethyl acetate (2 x 10 mL). The organic layers were combined and washed with saturated aqueous ammonium chloride (3 x 15 mL). The ammonium chloride washes were combined and back extracted with ethyl acetate (15 mL). The organic layers were combined, washed with brine/ 1 M hydrochloric acid (4:1 v/v) (15 mL), dried over sodium sulfate, filtered, and concentrated under reduced pressure to give the title compound, which was used in the next reaction without further purification. MS (APCI+) m/z 513.4 [M+H]+.

Statistics shows that 1-Bromo-2-cyclohexylethane is playing an increasingly important role. we look forward to future research findings about 1647-26-3.

Reference:
Patent; CALICO LIFE SCIENCES LLC; ABBVIE INC.; FARNEY, Elliot; SHIROODI, Roohollah, Kazem; XIONG, Zhaoming; ZHANG, Qingwei, I.; O’CONNOR, Matthew; HALVORSEN, Geoff; ZHAO, Hongyu; BAUMGARTNER, Christina; FROST, Jennifer, M.; KYM, Phil; ABBOTT, Jason, R.; BOGDAN, Andrew; ECONOMOU, Christos; WANG, Xueqing; (375 pag.)WO2019/246513; (2019); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

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. 454-79-5, name is 2-Bromo-5-(trifluoromethyl)aniline, This compound has unique chemical properties. The synthetic route is as follows., COA of Formula: C7H5BrF3N

Example 239 2-Mercapto-5-trifluoromethyl-benzothiazole (239) In analogy to the procedure of Chaudhuri, N. Synth. Commun. 1996, 26, 20, 3783, O-ethylxanthic acid, potassium salt (Lancaster, 7.5 g, 46.9 mmol) was added to a solution of 2-bromo-5-trifluoromethylphenylamine (Aldrich, 5.0 g, 20.8 mmol) in N,N-dimethylformamide (DMF, 30 mL). The mixture was heated to reflux for 4 hours. After cooling to room temperature, the mixture was poured into ice water and acidified with 2N HCl. The solid product was collected by filtration. Recrystalization from CHCl3/Hexanes gave 239 (4.5 g, 92%) as a white solid. 1H NMR (400 MHz, DMSO-d6) delta 14.00 (s, 1H), 7.94 (d, J=8.1 Hz, 1H), 7.62 (dd, J=8.4, 1.0 Hz, 1H), 7.48 (d, J=1.0 Hz, 1H). MS (M-H) 234.

According to the analysis of related databases, 454-79-5, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Tularik Inc.; US2003/139390; (2003); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Reference of 2044-08-8, 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. 2044-08-8, name is 1-Bromocyclohex-1-ene belongs to bromides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

Add 20 g (0.12 mol) of 1-bromo-1-cyclohexene to a three-necked flask under nitrogen atmosphere.34.7 g (0.14 mol) of pinacol borate and 2.0 g (6 mol%) of triphenylphosphine,2.6 g (3 mol%) of trans-bis(triphenylphosphine)palladium(II) dichloride,Potassium phenolate 24.6 g (0.19 mol) and anhydrous toluene 250 mL.After nitrogen substitution, the reaction was stirred at 50 C for 5 hours.The system was then cooled to room temperature and quenched with water.The reaction mixture was extracted with a benzene solvent and brine.The organic phase was dried over anhydrous magnesium sulfate. The dried mixture was filtered and concentrated under reduced pressure.Purification by silica gel column or distillation gave 21.9 g (yield: 85%) of cyclohexene-1-boronic acid pinacol.

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-Bromocyclohex-1-ene, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Yurui (Shanghai) Chemical Co., Ltd.; Zheng Xianzhe; (50 pag.)CN109384817; (2019); A;,
Bromide – Wikipedia,
bromide – Wiktionary

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. 103-64-0, name is (2-Bromovinyl)benzene, This compound has unique chemical properties. The synthetic route is as follows., Formula: C8H7Br

General procedure: beta-Bromostyrene (1.10 g, 6.0 mmol) in THF (7.5 mL) was added toa flask containing Mg turnings (0.17 g, 6.9 mmol) at room temperature. After being stirred for 1.5 h, N-formylpiperidine (0.34 g,3.0 mmol) in THF (2 mL) was added to the reaction mixture at 0C and the obtained mixture was stirred for 1 h at room temperature.Then, acetic anhydride (0.6 mL, 6.0 mmol) was added to the reactionmixture at 0 C and the mixturewas stirred for 0.5 h at roomtemperature. Then, aq NH3 (6 mL, 28-30%) and I2 (1.53 g, 6.0 mmol) were added to the reaction mixture at 0C and the obtainedmixture was stirred for 0.5 h at room temperature. Then, the reaction mixture was quenched with satd aq Na2SO3 and was extracted with CHCl3 (3*20 mL). The organic layer was dried over Na2SO4 and filtered. After removal of the solvent, the residue waspurified by short column chromatography on silica gel (eluent:hexane/ethyl acetate=9:1, v/v) to provide pure cinnamonitrile (0.32 g) in 83% yield.

According to the analysis of related databases, 103-64-0, the application of this compound in the production field has become more and more popular.

Reference:
Article; Ishii, Genki; Harigae, Ryo; Moriyama, Katsuhiko; Togo, Hideo; Tetrahedron; vol. 69; 5; (2013); p. 1462 – 1469;,
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. 17247-58-4, name is (Bromomethyl)cyclobutane, A new synthetic method of this compound is introduced below., Formula: C5H9Br

A solution of 12.3 g (83 mmol) of cyclobutylcarbinyl bromide (Aldrich) and 13.7 g (91 mmol) of sodium iodide in 150 mL of acetone was refluxed overnight and then cooled to room temperature. The inorganic solids were filtered off and the acetone and cyclopropylcarbinyl iodide (8.41 g, 46%) distilled off at ambient and 150 torr at 80 C., respectively. A solution of 4.0 g (21.98 mmol) of cyclobutylcarbinyl iodide in 30 mL of anhydrous diethyl ether (diethyl ether) cooled to -78 C. was cannulated into a solution of 17 mL (21.98 mmol) of 1.3M sec-butyl lithium in cyclohexanes and the solution was stirred for 5 minutes. To this mixture was cannulated a solution of 3.0 g (21.98 mmol) of freshly distilled sulfuryl chloride in 110 mL of hexanes cooled to -78 C., the mixture warmed to room temperature over 1 hour and was then carefully concentrated in vacuo. This mixture was redissolved in diethyl ether, washed once with some ice-cold water, dried (MgSO4), filtered, and concentrated carefully. This mixture was redissolved in 30 mL of THF, added dropwise to 500 mL of saturated NH3 in THF and was allowed to stir overnight. The mixture was concentrated in vacuo to a crude yellow solid and was recrystallized from the minimum amount of CH2Cl2 in hexanes with 1-2 drops of methanol to provide 1.39 g (42%) of cyclobutyl carbinylsulfonamide as a white solid. 1H NMR (CDCl3) delta 1.81-2.03 (m, 4H), 2.14-2.28 (m, 2H), 2.81-2.92 (m, 1H), 3.22 (d, J=7 Hz, 2H), 4.74 (br s, 2H); 13C NMR (CDCl3) delta 19.10, 28.21, 30.64, 60.93; MS m/e 148 (M-1)-. (Retention time: 1.73, method B), 818 (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; Hewawasam, Piyasena; Ding, Min; Sun, Li-Qiang; Scola, Paul Michael; US2007/10455; (2007); A1;,
Bromide – Wikipedia,
bromide – Wiktionary