Category: bromides-buliding-blocks

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. 108-85-0, name is Bromocyclohexane, A new synthetic method of this compound is introduced below., COA of Formula: C6H11Br

General procedure: Na2S·3H2O (0.291 g, 2.2 mmol) was addedto a magnetically stirred solution of an alkyl halide (2 mmol) and C2Cl6 or CCl4 (1.5 mmol) in PEG-200 (2 mL) at r.t. The stirring was continued until the starting halide was completely consumed (30-150 min). Next, the reaction mixture was diluted with H2O (1 mL) and extracted with EtOAc-hexane (1:1;4 × 2 mL). The organic extracts were combined, concentrated and purified by chromatography on silica gel. The desired disulfides were produced in excellent yields (Table 1).

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; Abbasi, Mohammad; Mohammadizadeh, Mohammad Reza; Moosavi, Hekmat; Saeedi, Narges; Synlett; vol. 26; 9; (2015); p. 1185 – 1190;,
Bromide – Wikipedia,
bromide – Wiktionary

Adding a certain compound to certain chemical reactions, such as: 452-92-6, name is 5-Bromo-2,4-difluoroaniline, 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 452-92-6, COA of Formula: C6H4BrF2N

General Procedure: Methyl 2-{[4-(chlorosulfonyl)-2,3-dimethylphenyl]oxy}propanoate (7) (4 g, 13.0 mmol) was dissolved in pyridine (10 mL). After 5 min, 3-bromo-2-chloroaniline (3.22 g, 15.6 mmol) was added. The reaction was complete within a few hours. The reaction mixture was then extracted using diethyl ether. The combined organic phases were washed with 1N HCl and brine, dried over sodium sulfate, filtered, and concentrated in vacuo to afford the title compound which was used without further purification.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 5-Bromo-2,4-difluoroaniline, and friends who are interested can also refer to it.

Reference:
Article; Evans, Karen A.; Shearer, Barry G.; Wisnoski, David D.; Shi, Dongchuan; Sparks, Steven M.; Sternbach, Daniel D.; Winegar, Deborah A.; Billin, Andrew N.; Britt, Christy; Way, James M.; Epperly, Andrea H.; Leesnitzer, Lisa M.; Merrihew, Raymond V.; Xu, Robert X.; Lambert, Millard H.; Jin, Jian; Bioorganic and Medicinal Chemistry Letters; vol. 21; 8; (2011); p. 2345 – 2350;,
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. 937046-98-5, name is 7-Bromopyrrolo[2,1-f][1,2,4]triazin-4-amine belongs to bromides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Recommanded Product: 937046-98-5

Intermediate 69A 7-( Prop- 1 -en-2-yl)pyrrolo[2, l-fj[l ,2,4]triazin-4-amine The starting material 7-bromopyrrolo[2, 1 -fj [ 1 ,2,4]triazin-4-amine was synthesized according to the procedure described in WO 2007/056170-A2 (Intermediate B). Under an argon atmosphere, 7-bromopyrrolo[2, 1 -f] [ 1 ,2,4]triazin-4-amine (426 mg, 2 mmol) and 4,4,5, 5-tetramethyl-2-(prop-l -en-2-yl)-l,3,2-dioxaborolane (420 mg, 2.5 mmol) were dissolved in a mixture of 1 ,2-dimethoxyethane (10 mL) and aqueous sodium carbonate solution (2 M, 4 mL). The reaction mixture was degassed, and 1 , 1 ‘-bis(diphenylphosphino)ferrocenepalladium(II) chloride (73 mg, 0.1 mmol) was added. After stirring at 90C overnight, the reaction mixture was diluted with ethyl acetate (40 mL), water (10 mL) was added, and the layers were separated. The aqueous layer was extracted with ethyl acetate (2 x 40 mL), and the combined organic layers were dried over sodium sulfate, filtered and concentrated. The residue was purified by flash chromatography (puriFlash, Interchim, cyclohexane/ethyl acetate 1 : 1 to 100% ethyl acetate gradient) to yield the title product as a slightly yellow solid. Yield: 304 mg (81 % of th.). HPLC (method 10): R, = 0.83 min; LC-MS (method 10): RT = 0.57 min; MS (ESIpos): m/z (%) = 1 75. 1 (100) [M+H]+. ? Iota NMR (400 MHz, 4J-DMSO): delta (ppm) = 2.15 (s, 3H), 5.22 (m, 1H), 6.30 (m, H I ). 6.73 (d, 1H), 6.91 (d, 1H), 7.69 (m, 1H), 7.91 (s, 1H).

The synthetic route of 937046-98-5 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; BAYER INTELLECTUAL PROPERTY GMBH; Bayer Pharma Aktiengesellschaft; KLAR, Juergen; VOEHRINGER, Verena; TELSER, Joachim; LOBELL, Mario; SUessMEIER, Frank; LI, Volkhart Min-Jian; BOeTTGER, Michael; GOLZ, Stefan; LANG, Dieter; SCHLEMMER, Karl-Heinz; SCHLANGE, Thomas; SCHALL, Andreas; FU, Wenlang; WO2013/4551; (2013); A1;,
Bromide – Wikipedia,
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955959-84-9, name is 4-(4-Bromophenyl)dibenzo[b,d]furan, belongs to bromides-buliding-blocks compound, is considered to be a conventional heterocyclic compound, which is widely used in drug synthesis. The chemical synthesis route is as follows. Quality Control of 4-(4-Bromophenyl)dibenzo[b,d]furan

[Example-of-Synthesis 1 (Synthesis of Compound H1) ]; Under an argon gas flow, 6.5 g of Intermediate 5, 9.5 g of Intermediate 12, 2.6 g of t-butoxy sodium (manufactured by Hiroshima Wako Co., Ltd.), 92 mg of tris (dibenzylideneacetone) dipalladium(0) (manufactured by SIGMA-ALDRICH Corn.), 42 mg of tri-tert-butylphosphine and 100 ml of dehydrated toluene were placed and the reaction was allowed to proceed at 80°C for 8 hours. The resultant solution was cooled down, added with 500 ml of water and filtered through sellite. The resultant filtrate was extracted with toluene, and the extract was dried over dehydrated magnesium sulfate. The dried substance was condensed under reduced pressure and the coarse product was subjected to column purification. The purified substance was re-crystallized with a use of toluene and after the resultant crystal was taken by filtration, the crystal was dried and as a result, 8.1 g of a pale yellow powder was obtained. The pale yellow powder was identified as Compound H1 from the result in accordance with the FD-MS analysis.

The synthetic route of 955959-84-9 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Idemitsu Kosan Co., Ltd.; EP2295421; (2011); A1;,
Bromide – Wikipedia,
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Synthetic Route of 698-19-1, 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. 698-19-1 name is 1-(2-Bromophenyl)-N-methylmethanamine, 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.

Preparation of ferf-butyl 2-bromobenzyl(methyl)carbamate (59). 58 59 A solution of compound 58 (2.0 g, 10.0 mmol) and Boc20 (2.29 g, 10.5 mmol) in THF (40 mL) was stirred at RT for 16 hours. The mixture was then concentrated in vacuo. The crude product was purified by flash column chromatography over silica gel, which was eluted with 10% EtOAc in heptanes, and yielded compound 59 as a colorless oil (2.8 g, 95% yield). 1H NMR (400 MHz, CDCI3) delta 7.54 (d, 1 H), 7.30 (t, 1 H), 7.13 (m, 2 H), 4.53 (br d, 2 H), 2.87 (br s, 3 H), 1.46 (br d, 9 H).

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 1-(2-Bromophenyl)-N-methylmethanamine, and friends who are interested can also refer to it.

Reference:
Patent; PFIZER INC.; BAILEY, Simon; BURKE, Benjamin, Joseph; COLLINS, Michael, Raymond; CUI, Jingrong, Jean; DEAL, Judith, Gail; HOFFMAN, Robert, Louis; HUANG, Qinhua; JOHNSON, Ted, William; KANIA, Robert, Steven; KATH, John, Charles; LE, Phuong, Thi, Quy; MCTIGUE, Michele, Ann; PALMER, Cynthia, Louise; RICHARDSON, Paul, Francis; SACH, Neal, William; WO2013/132376; (2013); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Electric Literature of 18599-22-9, 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 18599-22-9 as follows.

To a stirred solution of silver acetate (10 mg, 0.060 mmol) in glacial acetic acid (20 mL) at reflux temperature was added zinc powder (10 g, 153 mmol) in one portion, and the whole was stirred at that temperature for additional 30 seconds. After refluxing for 30 seconds, the flask was cooled by dipping in an ice-bath. The Zn-Ag couple formed was separated by vacuum filtration in the open-air, which was washed with Et2O several times, followed by drying under reduced pressure. The Zn-Ag couple separated was stored at room temperature under Ar atmosphere. See Figure S1 Preparation of CH2=CHCF2CF2ZnBr in DMF (2-Zn) In a two-necked round-bottomed flask, equipped with a teflon-coated stirrer bar, was placed Zn-Ag couple (0.66 g, 10 mmol) in DMF (5.0 mL). To the suspension was slowly dropwise added 4-bromo-3,3,4,4-tetrafluorobut-1-ene (1, 1.0 g, 5.0 mmol) at 0 C and the whole was stirred at that temperature for 30 min. The resultant was subjected to a short pad of celite and washed by Et2O three times. The filtrate was concentrated in vacuo to give the corresponding organozinc reagents 2-Zn in 86% NMR yield as a 0.70 M DMF solution (1,1,2,2-Tetrafluorobut-3-en-1-yl)zinc bromide in DMF (2-Zn) Yield: 86% (determined by 19F NMR); 19F NMR (CDCl3): 112.10 (brs, 2F, CF2CH), 120.23 (brs, 2F, CF2Zn).

According to the analysis of related databases, 18599-22-9, the application of this compound in the production field has become more and more popular.

Reference:
Article; Tamamoto, Ken; Yamada, Shigeyuki; Konno, Tsutomu; Beilstein Journal of Organic Chemistry; vol. 14; (2018); p. 2375 – 2383;,
Bromide – Wikipedia,
bromide – Wiktionary

4549-33-1, name is 1,9-Dibromononane, belongs to bromides-buliding-blocks compound, is considered to be a conventional heterocyclic compound, which is widely used in drug synthesis. The chemical synthesis route is as follows. Application In Synthesis of 1,9-Dibromononane

EXAMPLE 4 N, N’-Nonane-1, 9-diyl-bis-pyridinium Dibromide (bPNB).; 1,9-Dibromononane (mmol) was added to a solution (30 mL) of dry pyridine, and the solution heated for 24 hours at 65C. The resulting precipitate was filtered, and the product washed five times with dry diethyl ether. The resulting clear liquid was isolated in a 87% yield. ‘H NMR (300 MHz, DMSO-D6) 5 9.17 (2H, d, C2&C6-H), 8.61 (1H, t, C4-H), 8. 18 (2H, t, C3&C5-H), 4.63 (2H, t, C’1-CH2), 1.89 (2H, m, C’2-CH2), 1.22 (5H, m, C’3-5-CH2) ; 13C NMR (75 MHz, DMSO-D6) 8 145.3, 144.5, 127.9, 60.5, 30.7, 28.4, 28.2, 25.3.

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

Reference:
Patent; UNIVERSITY OF KENTUCKY RESEARCH FOUNDATION; WO2005/66129; (2005); A2;,
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. 1647-26-3, name is 1-Bromo-2-cyclohexylethane, A new synthetic method of this compound is introduced below., Recommanded Product: 1-Bromo-2-cyclohexylethane

Step 1: Preparation of ethyl 9-(2-c> elohexyIeth()xy)-6-ethyI-10-methoxy-2-oxo-6,7- dihydrobenzo [a] qiiinolizine-3-earbox late A mixture of ethyl 6-ethyl-9-hydroxy-10-methoxy-2-oxo-6,7-dihydroberizo[a]quinolizme- 3-carboxylate (50 mg, 0.15 mmol), 2 – b ro mo e t h y 1 c y c 1 o h e x a n e (57 mg, 0.3 mmol) and K2CO3 (62 mg, 0.45 mmol) in DMF (2 ml.) was stirred at 80 C for 2 hours. Water was added and the mixture was extracted with ethyl acetate. The organic phase was dried over anhydrous Na^SOj and then concentrated in vacuo to give crude ethyl 9-(2-cyclohexylethoxy)-6-ethyl- 10-methoxy- 2-0X0-6, 7-dihydrobenzo[a]qiiinolizine-3-carboxylate (69 mg) which was used in the next step without purification.

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; F. HOFFMANN-LA ROCHE AG; HOFFMANN-LA ROCHE INC.; HAN, Xingchun; JAVANBAKHT, Hassan; JIANG, Min; LIANG, Chungen; WANG, Jianping; WANG, Yongguang; WANG, Zhanguo; WEIKERT, Robert James; YANG, Song; ZHOU, Chengang; WO2015/113990; (2015); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

These common heterocyclic compound, 67344-77-8, name is 1-(3-Bromophenyl)-N-methylmethanamine, 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. SDS of cas: 67344-77-8

To a solution of 1-(3-bromophenyl)-N-methylmethanamine (12.0 g) and N-(tert-butoxycarbonyl)glycine (11.5 g) in dichloroethane (80 ml) were added HOBt (9.7 g) and WSC hydrochloride (13.7 g), followed by stirring at room temperature overnight. To the reaction mixture was added a saturated aqueous sodium hydrogen carbonate solution, followed by extraction with CHCl3. The mixture was dried over Na2SO4 and then concentrated under reduced pressure. The obtained residue was purified by silica gel column chromatography (CHCl3/MeOH) to obtain tert-butyl {2-[(3-bromobenzyl)amino]-2-oxoethyl}carbamate (21.3 g).

The synthetic route of 1-(3-Bromophenyl)-N-methylmethanamine has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Astellas Pharma Inc.; US2012/184520; (2012); 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. 2635-13-4, name is 5-Bromobenzo[d][1,3]dioxole, A new synthetic method of this compound is introduced below., Product Details of 2635-13-4

General procedure: A 25 mL Schlenk tube was charged with Cu2O (0.05 mmol), ArX (0.5 mmol), NHR1R2 (0.75 mmol), NaOH (1 mmol), TBAB (0.1 mmol), L2 (0.1 mmol) and H2O/EtOH (1 mL, 1/1, v/v). The mixture was stirred at 120 C for 12 h. The reaction mixture was extracted with ethyl acetate (3 10 mL), washed with water and brine, dried over anhydrous Na2SO4, and concentrated in vacuo. The residue was purified by flash column chromatograph on silica gel(ethyl acetate/petroleum ether as the eluent) to provide the target products 3a-3w and 6.

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; Xie, Jian-Wei; Yao, Zhen-Bin; Wang, Xiao-Chuang; Zhang, Jie; Tetrahedron; vol. 75; 27; (2019); p. 3788 – 3792;,
Bromide – Wikipedia,
bromide – Wiktionary