Tag: M.W=300-400

These common heterocyclic compound, 10016-52-1, name is 2,8-Dibromodibenzo[b,d]furan, 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. Recommanded Product: 2,8-Dibromodibenzo[b,d]furan

General procedure: 3.26 g of 2,8-dibromodibenzofuran, 1.9 g of pyridin-2-ol, 0.2 g of CuI, 0.2 g of 1,10-phenanthroline, and 6.3 g of K3PO4 were added to 200 mL of dimethylformamide (DMF) and stirred at a temperature of 160 C. for 24 hours. After cooling, 400 mL of a mixed solution including brine ice was added thereto, and a reaction mixture was precipitated, filtered, and washed with water. An organic layer obtained therefrom by washing the reaction mixture with ethyl acetate and water three times was dried by using MgSO4 and dried under reduced pressure. Column chromatography was used to obtain 1.77 g (yield: 50%) of Intermediate 1-1.

The synthetic route of 2,8-Dibromodibenzo[b,d]furan has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Samsung Display Co., Ltd.; SIM, Munki; KO, Soobyung; KIM, Sungbum; PARK, Junha; AHN, Heechoon; LEE, Hyoyoung; JEON, Mina; JUN, Mieun; HAN, Junghoon; KIM, Youngkook; HWANG, Seokhwan; (93 pag.)US2019/296253; (2019); A1;,
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Synthetic Route of 4101-68-2, These common heterocyclic compound, 4101-68-2, name is 1,10-Dibromodecan, 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.

Under nitrogen atmosphere, compound 7 (1.23 g, 1.65 mmol), 1,10-dibromodecane (2.97 g, 9.9 mmol), potassium hydroxide (0.43 g, 6.6 mmol), tetrabutylammonium bromide , 0.495 mmol) was added to dichloromethane (10 ml) and water (6.5 ml), and the mixture was stirred at room temperature for 24 hours. The mixture was allowed to stand for several minutes. The aqueous layer and the organic layer were separated, and methanol (30 ml) was added to the organic layer. The precipitate was filtered and purified by silica gel column chromatography (eluent ethyl acetate / petroleum ether, volume ratio 1: 30-1: 20) to give a colorless solid (1.41 g) in 89% yield.

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

Reference:
Patent; Guilin University of Technology; Kong, Xiangfei; Wang, Guixia; Xia, Liting; Su, Jian; Zhang, Haifeng; (19 pag.)CN105541616; (2016); A;,
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Reference of 10546-67-5, 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. 10546-67-5, name is 2,6-Dibromo-4-(tert-butyl)aniline belongs to bromides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

The aniline (75 g, 67 mol) was dissolved in DMF (37 mL), NBS added (25 grams; 142 mrnol) and the solution stirred at RT overnight. The solution was diluted with aqueous NaOH (I N, 370 mL) followed by aqueous/EtOAc work-up to afford the titled compound. The crude oil was dissolved in DMF (24 mL), added dropwise to a 70 0C solution of isoamyl nitrite (1 1.8 g, 101 mmol) in DMF (24 mL) and stirred for 30 minutes. The solution was cooled to RT, diluted with water (700 mL), acidified with AcOH, followed by aqueous/EtOAc work-up and silica gel chromatography (hexanes, neat) to afford the titled compound.

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, 2,6-Dibromo-4-(tert-butyl)aniline, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; MERCK & CO., INC.; WO2007/64553; (2007); A2;,
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Electric Literature of 3344-70-5, These common heterocyclic compound, 3344-70-5, name is 1,12-Dibromododecane, 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: All compounds were prepared according to previously described procedures [16,17]. Briefly, a phenol derivative (0.015 mol) and a dibromoalkane (0.0075 mol) were dissolved in a mixture of ethanol and water (9/1) containing an alkaline hydroxide (0.015 mol). The mixture was heated under microwave irradiation in an Initiator? Biotage oven for 20 min at 120 ¡ãC. After cooling, the precipitate was filtered and thoroughly washed with water, ethanol and ether.

The synthetic route of 3344-70-5 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Cappoen, Davie; Forge, Delphine; Vercammen, Frank; Mathys, Vanessa; Kiass, Mehdi; Roupie, Virginie; Anthonissen, Roel; Verschaeve, Luc; Vanden Eynde, Jean Jacques; Huygen, Kris; European Journal of Medicinal Chemistry; vol. 63; (2013); p. 731 – 738;,
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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. 18648-66-3, name is 2-(4-Bromophenyl)-1,1-diphenylethylene, A new synthetic method of this compound is introduced below., Quality Control of 2-(4-Bromophenyl)-1,1-diphenylethylene

Under the atmosphere of argon, 4-(2,2-diphenylvinyl)bromobenzene (10 g, 30 mmole, 3 eq) was dissolved into a mixed solvent composed of anhydrous toluene (45 ml) and anhydrous THF (45 ml), and the resultant solution was cooled to -20C in a dry ice/methanol bath. To the cooled solution, a hexane solution of n-butyllithium (1.59 mmole/liter, 20 ml, 32 mmole, 1.06 eq) was added, and the obtained solution was stirred at -20C for 1 hour. To the resultant solution, 2-(2-phenyl-2-)propylanthraquinone (3.5 g, 11 mmole) was added, and the obtained mixture was stirred at the room temperature for 3 hours and then left standing for one night. To the resultant reaction mixture, a saturated aqueous solution of ammonium chloride (50 ml) was added. The organic layer was separated, washed with a saturated aqueous solution of sodium chloride and dried with magnesium sulfate. After the solvent was removed by distillation, the product was purified in accordance with the column chromatography (silica gel; hexane+50% dichloromethane, dichloromethane and finally dichloromethane+3% methanol), and a light yellow amorphous solid was obtained (5.7 g; the yield: 67%).

The synthetic route of 18648-66-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; IDEMITSU KOSAN CO., LTD.; EP1440959; (2004); A1;,
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Reference of 4101-68-2,Some common heterocyclic compound, 4101-68-2, name is 1,10-Dibromodecan, molecular formula is C10H20Br2, 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.

1.23 g of compound 3, 2.97 g of 1,10-dibromodecane, 0.43 g of potassium hydroxide and 0.16 gTetrabutylammonium bromide was added to 10 ml of methylene chloride and 6.5 ml of water, and the mixture was stirred at room temperature for 24 hours under a nitrogen atmosphere.Washed twice with 30 ml of water, washed with 15 ml of saturated brine, the organic layer was separated,After drying with anhydrous sodium sulfate, the solvent was removed by rotary evaporator,Purification with 200-300 mesh silica gel column chromatography (eluent is ethyl acetate / petroleum ether, volume ratio of 1: 30-1:20) to give 1.41 g of compound 4 as a colorless solid in 89% yield

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

Reference:
Patent; Guilin University of Technology; Kong, Xiangfei; Dai, Shengping; Zhang, Laiqi; Liao, Peihai; Wang, Guixia; (10 pag.)CN106117225; (2016); A;,
Bromide – Wikipedia,
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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. 4101-68-2, name is 1,10-Dibromodecan belongs to bromides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. name: 1,10-Dibromodecan

Compound 3 (713 mg, 0.5 mmol) was dissolved in anhydrous toluene (5 mL). 1,10-Dibromodecane (450 mg, 1.5 mmol), a catalytic amount of tetrabutylammonium hydrogen sulfate (TBAHS) (0.05 mmol), and KOH (1.5 mmol) were added into this solution subsequently. This reaction mixture was stirred at room temperature under N2 gas overnight and then concentrated under reduced pressure. The residue was purified by flash chromatography (elution with a gradient of hexanes/ethyl acetate from 10:1 to 4:1) to give the desired product as a white solid. Yield: 666 mg (81%). 1H NMR (300 MHz, chloroform-d) delta 5.23 (d, J = 3.1 Hz, 1H, anomeric H), 5.19 – 5.13 (m, 1H, anomeric H), 4.33 – 4.22 (m, 1H), 4.18 (d, J = 10.2 Hz, 1H), 4.09 (d, J = 5.8 Hz, 1H), 3.87 – 3.10 (m, 17H), 2.48 (d, J = 11.4 Hz, 1H), 2.07 – 1.96 (m, 1H), 1.92 – 1.80 (m, 2H), 1.57 – 1.50 (m, 1H), 1.48 – 1.40 (m, 45H), 1.39 – 1.18 (m, 14H), 1.12 – 1.00 (m, 1H), 0.99 – 0.82 (m, 36H), 0.22 – -0.03 (m, 24H). 13C NMR (75 MHz, chloroform-d) delta 155.63, 155.55, 154.85, 154.77, 154.59, 97.87 (anomeric C), 96.54 (anomeric C), 85.78, 79.95, 79.63, 79.39, 79.24, 79.11, 77.45, 75.31, 73.37, 72.69, 71.56, 68.07, 66.88, 63.16, 63.13, 57.32, 50.57, 48.97, 48.38, 41.73, 36.66, 35.97, 35.90, 35.68, 33.99, 33.80, 32.88, 30.66, 30.43, 29.98, 29.72, 29.70, 29.65, 29.56, 29.47, 29.38, 28.80, 28.66, 28.53, 28.42, 28.20, 26.15, 26.02, 26.01, 25.80, 24.70, 23.45, 18.51, 18.35, 18.12, 17.93, -3.39, -3.77, -4.18, -4.86, -4.92, -5.06, -5.14, -5.20. MS (ESI) m/e calcd for C77H152BrN5O19Si4Na [M+Na]+: 1667.3, found: 1667.4.

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

Reference:
Article; Yang, Xuan; Ammeter, Derek; Idowu, Temilolu; Domalaon, Ronald; Brizuela, Marc; Okunnu, Oreofe; Bi, Liting; Guerrero, Yanelis Acebo; Zhanel, George G.; Kumar, Ayush; Schweizer, Frank; European Journal of Medicinal Chemistry; vol. 175; (2019); p. 187 – 200;,
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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. 201138-91-2, name is 4,6-Dibromodibenzo[b,d]furan, A new synthetic method of this compound is introduced below., Safety of 4,6-Dibromodibenzo[b,d]furan

A mixture of 13 g (40 mmol) of 4,6-dibromobenzofuran, 11.3 g (40 mmol) of bis(4-tert-butylphenyl)amine, 0.9 g (0.8 mmol) of Pd2(dba)3, 1.2 g (0.6 mmol) of tri-tert-butylphosphine, 5.0 g (52 mmol) of sodium tert-butoxide, and 150 ml of toluene was placed under nitrogen, and then heated and stirred at 70 C. for 24 hrs. After the reaction finished, the mixture was allowed to cool to room temperature. The solution was extracted with 100 ml of ethyl acetate and 300 ml of water. The organic layer was dried with anhydrous magnesium sulfate and the solvent was evaporated under reduced pressure. The residue was purified by column chromatography on silica to give product (16 g, 30.4 mmol, 76%).

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; LUMINESCENCE TECHNOLOGY CORPORATION; Yen, Feng-Wen; Chuang, Li-Chieh; Huang, Tsun-Yuan; (76 pag.)US2019/348609; (2019); A1;,
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Related Products of 18648-66-3,Some common heterocyclic compound, 18648-66-3, name is 2-(4-Bromophenyl)-1,1-diphenylethylene, molecular formula is C20H15Br, 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.

(2,3-dihydrothieno[3,4-b][1,4]dioxin-5-yl)trimethylstannan (0.81 g 2.66 mmol), 1-bromo-4-(2,2-diphenylvinyl)benzene (a compound of the Chemical Formula 2r) (1.7 g, 3.2 mmol), and Pd(PPh3)4 (0.15 g, 0.13 mmol) were dissolved in toluene (40 ml), and then refluxed under nitrogen atmosphere for 8 hours. Subsequently, an organic layer was extracted with methylene chloride and water and distilled, and column chromatography was performed (eluent-MC:Hx=1:4) to synthesize a compound of the Chemical Formula 4r.1H NMR (CDCl3): [ppm]=4.68 (s, 2H), 4.72 (s, 2H), 6.71 (s, 1H), 6.96 (s, 1H), 7.08 (s, 1H), 7.18 (m, 4H), 7.40 (m, 2H), 7.48 (m, 6H), 7.56 (d, 3JHH=8.8 Hz, 2H).

The synthetic route of 18648-66-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Dongjin Semichem Co., Ltd.; US2011/94588; (2011); A1;,
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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. 2789-89-1, name is 1,2-Bis(4-bromophenyl)ethyne, A new synthetic method of this compound is introduced below., HPLC of Formula: C14H8Br2

To a 13 ¡Á 150 mm test tube equipped with magnetic stir bar were added [RhCp*(CH3CN)3](SbF6)2 (6.6mg, 4 mol %), NaOAc (32.8mg, 0.4 mmol, 2 equiv) and 2a-2o (0.3 mmol, 1.5 equiv). The test tube was sealed with a rubber septum and removed from the glove-box. The solution of 1a-1r (0.2 mmol, 1 equiv)in EtOH (2 mL) was injected into the test tube via syringe. The reaction mixture was placed in a preheated oil bath (60 ) for 12 h. Then the reaction mixture was concentrated in vacuo, the residue was dissolved in methylene chloride and purified by column chromatography (silica gel, n-hexane/EtOAc =20/1). 1-Methyl-3,4-diphenylisoquinoline (3aa): The title compound was obtained as white crystal in 91% yield (54.2 mg). 1H NMR (400 MHz, CDCl3) delta 8.24 – 8.16(m, 1H), 7.66 (m, 1H), 7.63 – 7.55 (m, 2H), 7.41 – 7.28 (m, 5H), 7.26 – 7.12 (m,5H), 3.09 (s, 3H). 13C NMR (101 MHz, CDCl3) delta 157.78, 149.37, 140.90, 137.56,136.06, 131.44, 130.32, 130.04, 129.29, 128.24, 127.66, 127.18, 127.01, 126.62,126.29, 126.19, 125.60, 22.73. HRMS (EI) calcd. for C22H17N: [M]+, 295.1361. Found: m/z 295.1358.

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; Chu, Benfa; Fang, Lili; Guo, Shan; Qi, Bing; Shi, Pengfei; Wang, Qi; Zhu, Jin; Tetrahedron Letters; (2020);,
Bromide – Wikipedia,
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