Category: bromides-buliding-blocks

Reference of 327-75-3, A common heterocyclic compound, 327-75-3, name is 1-Bromo-2,4-bis(trifluoromethyl)benzene, molecular formula is C8H3BrF6, 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.

Intermediate 33. 2-(2,4-Bis-trifluoromethyl-phenoxy)-ethylamine. [00136] Step A:; (2-Hydroxy-ethyl) -carbamic acid tert-butyl ester (0.2 mL, 1.29 mmol) is dissolved in 3 mL dry dimethyl-acetamide. 2-Potassium-1,1,1,3,3,3-hexamethyl- disilazane (0.52 g, 2.6 mmol, 2 equiv. ) is added, followed by 1-bromo-2,4-bis- trifluoromethyl-benzene 31 (0.26 mL, 1.5 mmol, 1.2 equiv. ). The mixture is stirred at 60C under nitrogen for 18 hours. The mixture is cooled, diluted with 50 mL water and extracted with dichloromethane (3 x 50 mL). The combined organic extracts are washed with water and 10% aqueous citric acid, dried over Na2S04 and concentration. Silica gel chromatography (5% to 25% ethyl acetate in hexanes) yielded [2-(2,4-Bis-trifluoromethyl- phenoxy) -ethyl]-carbamic acid tert-butyl ester 32 as a colorless, mobile oil: ‘H-NMR (400 MHz, CDC13) 8 = 7.61 (s, 1H), 7.00 (d, J = 8 Hz, 1H), 6.76 (d, J = 8 Hz, 1H), 5.10 (s, 1H), 4.26 (t, J = 4 Hz, 2H), 3.65 (m, 2H), 1.45 (s, 9H). 19F-NMR (376 MHz, CDC13) 8 =-61.5, – 62.0. No molecular ion could be obtained; a loss of tert-butyl group is observed: MS calculated for C11H10F6NO3 (M+H+-C4H8) 318.1, found 318.3.

The synthetic route of 327-75-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; IRM LLC; WO2005/113519; (2005); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Related Products of 68322-84-9, These common heterocyclic compound, 68322-84-9, name is 2-Bromo-1-fluoro-4-(trifluoromethyl)benzene, 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.

j003201 A flask was charged with t-butyl 4-aminopiperidine-1-carboxylate (416 mg, 2.06 mmol, 2.00 equiv), 2-bromo-1-fluoro-4-(trifluoromethyl)benzene (250 mg, 1.03 mmol, 1.00 equiv), DIPEA (403 mg, 3.09 mmol, 3.00 equiv), and dimethyl sulfoxide (10 mL), as described in Example 1, Step 5. The residue was chromatographed on a silica gel column to provide 420 mg (96% yield) of t-butyl 4-((2-bromo-4-(trifluoromethyl)phenyl)amino)piperidine- 1 -carb oxylate as a yell ow oil. LCMS (ESI, m/z): 423 [M+H].

The synthetic route of 68322-84-9 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; ABIDE THERAPEUTICS, INC.; GRICE, Cheryl A.; WEBER, Olivia D.; BUZARD, Daniel J.; SHAGHAFI, Michael B.; WIENER, John J. M.; CISAR, Justin S.; DUNCAN, Katharine K.; (324 pag.)WO2018/217809; (2018); 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. 626-40-4, name is 3,5-Dibromoaniline, This compound has unique chemical properties. The synthetic route is as follows., Formula: C6H5Br2N

A solution of 3 (0.7 g, 3.83 mmol) in MeOH (10 mL) was treated with 7 (1.0 g, 4 mmol), refluxed for 12 h, and cooled to roomtemperature to afford 8 (1.6 g, 97%), white crystals, mp 169-170C (MeOH), []D20 -66.72 (c 0.069, DMSO). IR spectrum(, cm-1): 3367-3073 (), 1574 (Ar), 1518 (NH), 1176, 1073 (–), 892 (-, -anomer), 668 (-Br). C12H15Br2NO5.1 NMR spectrum (400 MHz, CDCl3, , ppm, J/Hz): 3.1 (2H, m, -3, 5), 3.17 (3, d, J = 5.2, a), 3.24 (2H, m, -2, 4),3.40-3.65 (1H, ddd, J = 11.8, 5.8, 1.9, H-1), 4.18 (1H, q, J = 5.2, aOH), 4.36 (1H, t, J = 8, H-6), 4.52 (1H, t, J = 5.8, 1-OH),4.96, 4.97 (2H, dd, J = 5.3, 5.5, 3, 5-OH), 5.05 (1H, d, J = 4.8, 4-OH), 6.86 (2H, d, J = 7.6, H-8, 12), 6.89 (1H, d, J = 7.8, NH),6.95 (1H, t, J = 1.6, -10). 13C NMR spectrum (100 MHz, CDCl3, , ppm): 49.1 (a), 61.3 (t, -1), 70.7 (d, -3), 73.5 (d,-5), 77.8 (d, -4), 77.9 (d, -2), 84.5 (d, -6), 115.1 (d, -8, d, -12), 121.5 (d, -10), 123.1 (s, -9, s, -11), 150.7 (s, -7).

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 626-40-4.

Reference:
Article; Makaev; Pogrebnoi; Chemistry of Natural Compounds; vol. 52; 1; (2016); p. 86 – 89; Khim. Prir. Soedin.; (2015); p. 80 – 83,4;,
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.

the intermediate 14 (1.30g, 2mmol), intermediate 5 (4.44g, 12mmol), four (triphenylphosphine) palladium (280 mg, 0 . 24mmol) and sodium carbonate (1.06g, 10mmol) added to the reaction in the bottle, the substitute gas three times, under the protection of nitrogen injection THF (80 ml) and H2 O (20 ml), 80 °C heating reflux reaction 24h. Water quenching reaction, by methylene chloride extraction, after concentrating makes the powder, eluent for (petroleum ether/dichloromethane=10/1) column, to obtain the final product TPE – TB, yield 85percent.

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, 1,1,2,2-Tetrakis(4-bromophenyl)ethene, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; South China University of Technology; Tang Benzhong; Chen Long; Zhao Zujin; Qin Anjun; Hu Rongrong; (18 pag.)CN104031077; (2017); B;,
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. 955959-84-9, name is 4-(4-Bromophenyl)dibenzo[b,d]furan, A new synthetic method of this compound is introduced below., Recommanded Product: 955959-84-9

To a round bottom flask was added 4- (4-bromophenyl) dibenzofuran (1.23 g, 3.8 mmol), aminobiphenyl (0.71 g, 4.19 mmol)sodium tert-butoxide (0.512 g, 5.33 mmol),tris (dibenzylideneacetone) dipalladium (0) (0.07 g, 0.076 mmol) was dissolved in 50 ml of toluene. tri-tert-butylphosphine (0.03 g, 0.15 mmol) was added and the mixture was refluxed for 24 hours.After confirming with HPLC and LC-MASS, the reaction was terminated. After removal of the solvent, it was extracted with MC / H2O. column (EA: Hex = 1: 4) and reprecipitated with MC / hexane. Vacuum drying and sublimation purification were conducted to obtain a solid compound (1.25 g, yield = 80%).

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; LG Display Co., Ltd.; Choi Hye-ok; Lee Seung-jae; Pin Jong-gwan; Seo Bo-min; (39 pag.)KR2018/44695; (2018); A;,
Bromide – Wikipedia,
bromide – Wiktionary

Electric Literature of 49764-63-8, A common heterocyclic compound, 49764-63-8, name is 4,5-Dibromobenzene-1,2-diamine, molecular formula is C6H6Br2N2, 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.

A mixture of 100 ml of toluene, 10 g (0.036 mol) of the compound of example 12.3, 9.65 g (0.079 mol) of phenylboronic acid, 10 g of potassium carbonate and 1 .05 g of tetrakistriphenylphosphinepalladium was heated at 70C for 5 h. Then, the reaction mixture was mixed with water. The phases were separated to give 10.7 g of a crude product which was purified by column chromatography (toluene) to give 8.1 g (79%)

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; BASF SE; Koeneman, Martin; Materan, Gabriele; Bagain, Plast Gerhard; Ivanovic, Sorin; St., Robert; (100 pag.)KR2016/38052; (2016); A;,
Bromide – Wikipedia,
bromide – Wiktionary

Reference of 327-51-5, 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. 327-51-5, name is 1,4-Dibromo-2,5-difluorobenzene, This compound has unique chemical properties. The synthetic route is as follows.

Under argon stream, 1,2-dimethylimidazole (385 mg, 4.0 mmol), 1,4-dibromo-2,5-difluorobenzene (272 mg, 1.0 mmol)Potassium acetate (393 mg, 4.0 mmol) and palladium acetate (11 mg, 0.05 mmol) were suspended in dimethylacetamide (DMAc, 5.0 mL) and stirred at 150 C. for 48 hours. After allowing to cool, water was added to the reaction mixture, the precipitated solid was collected by filtration,Washing with water yielded the desired 1,4-bis(1,2-dimethylimidazol-5-yl)-2,5-difluorobenzene as a milky white solid (198 mg, 66%).

The chemical industry reduces the impact on the environment during synthesis 1,4-Dibromo-2,5-difluorobenzene. I believe this compound will play a more active role in future production and life.

Reference:
Patent; Tosoh Corporation; Sagami Chemical Research Institute; Aihara, Hidenori; Yamagata, Takuya; Hachiya, Hitoshi; Watanabe, Makoto; Fukuda, Takashi; Ueda, Saori; Miyashita, Masato; (64 pag.)JP2018/168149; (2018); A;,
Bromide – Wikipedia,
bromide – Wiktionary

10485-09-3, name is 2-Bromoindene, 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. Recommanded Product: 10485-09-3

Under an argon atmosphere, a solution of zinc chloride g, 28.0 mmol) in tetrahydrofuran suspension (5 mL) was added with a solution of isopropyl magnesium bromide in tetrahydrofuran (0.78 M, 30.7 mL) at 0 C., and the resultant was stirred at the same temperature for 1 hour. Then a solution of tetrakistriphenyl phosphine palladium (800 mg, 0.70 mmol) and 2-bromoindene (3.87 g, 20.0 mmol) in tetrahydrofuran (10 mL) was added thereto, and the resultant was further stirred at the same temperature for 16 hours. The reaction solution was added with a saturated aqueous solution of ammonium chloride, and extracted with diethyl ether. The organic layer was dried over anhydrous sodium sulfate, concentrated in vacuo, and the resultant residue was purified using silica-gel chromatography (hexane). 2-Isopropylindene (2.25 g, 71.1%) was obtained as a colorless oil.1H-NMR (400 MHz, CDCl3) delta; 1.22 (d, J=6.6 Hz, 6H), 2.77 (septet, J=6.6 Hz, 1H), 3.30 (s, 2H), 6.50 (s, 1H), 7.10-7.34 (m, 4H).

The synthetic route of 10485-09-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; KOWA COMPANY, LTD.; US2010/22572; (2010); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Electric Literature of 13633-25-5,Some common heterocyclic compound, 13633-25-5, name is 1-Bromo-4-phenylbutane, molecular formula is C10H13Br, 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.

lambda/-{2-r(3-phenylbutoxyphenylVphenyl- aminolethvDacetamide (5i): A mixture of lambda/-(3-hydroxyphenyl)aniline (2.7 mmol) and 1-bromo-4-phenylbutane (2.02 mmol) was refluxed for 5 h in a 10% ethanol solution of KOH. The reaction mixture was cooled to room temperature, poured into water and extracted three times with EtOAc. The combined organic phases were washed with brine, dried (Na2SO4) and evaporated under reduced pressure to provide a residue which was purified by flash chromatography (silica gel; cyclohexane/EtOAc, 8:2 as eluent). Yield lambda/-(3-phenylbutoxyphenyl)-aniline (3i): 86%; oil; EI-MS 317 (M+), 91 (100); 1H-NMR (CDCI3): delta 1.83 (m, 4H), 2.68 (m, 2H), 3.96 (m, 2H), 5.75 (br, 1 H), 6.46-7.38 (m, 14H).

The synthetic route of 13633-25-5 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; MCGILL UNIVERSITY; UNIVERSITA DEGLI STUDI DI PARMA; UNIVERSITA DEGLI STUDI DI MILANO; UNIVERSITA DEGLI STUDI DI URBINO; WO2007/79593; (2007); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Related Products of 10016-52-1, The chemical industry reduces the impact on the environment during synthesis 10016-52-1, name is 2,8-Dibromodibenzo[b,d]furan, I believe this compound will play a more active role in future production and life.

The second scheme: to 250 ml three-mouth bottle adding 2.36g (3.8 × 10-3Mol) precursor 3 (through the implementation of example three preparation) and 0.5g (1.53 × 10-3Mol) 2, 8 – dibromodiphenyl benzofuran, adding 100g toluene. Opening stirring, system for the picture and the turbid, N2Replacement system 10min. In the system by adding 0.37g (3.84 × 10-3Mol) tertiary butyl alcohol sodium, 0.045g (6.14 × 10-5Mol) Pd (dppf) Cl2And 0.025g (1.24 × 10-4Mol) tri-butyl phosphine, 110 C reaction 20 hours. The said technological, cooling to 20 – 25 C, the reaction liquid filtration, filtrate directly filtering of the silica gel column, eluting with toluene, the solvent under reduced pressure, the crude product shall be light brown red foam. In the above-mentioned crude product is added n-hexane and toluene recrystallization (mass ratio of 4:1), gain the light yellow powdery product 1.7g, yield: 65%.

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, 2,8-Dibromodibenzo[b,d]furan, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; CECEP Wanrun Co., Ltd.; Ren Huicai; Pang Maoyin; Yang Fushan; Tian Shaozhen; Shi Rujin; Hu Baohua; (14 pag.)CN105153085; (2017); B;,
Bromide – Wikipedia,
bromide – Wiktionary