Tag: M.W=300-400

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 955959-84-9 as follows. COA of Formula: C18H11BrO

In a 250mL flask, 4-(4′-bromophenyl)dibenzo[b,d]furan (10g) and tetrahydrofuran (90mL) were mixed and stirred under nitrogen atmosphere and cooled to -78°C. At -78°C, n-butyllithium (18.8ml, 2.5M in n-hexane) was added and stirred for 2 hours. After 2 hours, trimethyl borate (16g) was added and the reaction was equilibrated to room temperature overnight. The reaction was monitored by thin layer chromatography. Upon completion of the reaction, 2N hydrochloric acid solution (60mL) was added and stirred for 1 hour. It was quenched with water (50mL) and extracted with ethyl acetate (70mL). The organic layer was extracted with water (3x50mL) and dried over anhydrous sodium sulfate. Following this, the ethyl acetate layer was evaporated to dryness under vacuum rotavap to get 4-(dibenzofuran-4-yl)phenylboronic acid (5g).

According to the analysis of related databases, 955959-84-9, the application of this compound in the production field has become more and more popular.

Reference:
Patent; e-Ray Optoelectronics Technology Co., Ltd.; Ban, Ruman; Huang, Helong; Yao, Zhengcong; Xie, Bowei; Chen, Huixu; (34 pag.)CN105585555; (2016); 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 3344-70-5 as follows. Recommanded Product: 3344-70-5

General procedure: A dibromoalkane (1 equiv.) and sodium azide (3 equiv.) were dissolved in 4 : 1 DMF/H2O (15 mL). The mixture was irradiated in a CEM microwave reactor at 125oC (200 W, 200 psi) for 3 h. The reaction mixture was then cooled to room temperature, and 2-ethynylpyridine (2 equiv.), sodium ascorbate (0.5 equiv.), and CuSO4*5H2O (0.4 equiv.) were added to the reaction mixture. The mixture was stirred at room temperature for 12 h. The suspension was partitioned between aqueous 0.1M NH4OH/ethylenediaminetetraacetic acid (EDTA) (100 mL) and CH2Cl2 (100 mL), and the layers were separated. The organic phase was washed with water (100 mL) and brine (100 mL), dried over MgSO4, and the solvent was removed under reduced pressure to provide the ligands as off-white solids.

According to the analysis of related databases, 3344-70-5, the application of this compound in the production field has become more and more popular.

Reference:
Article; Kumar, Sreedhar V.; Lo, Warrick K. C.; Brooks, Heather J. L.; Hanton, Lyall R.; Crowley, James D.; Australian Journal of Chemistry; vol. 69; 5; (2016); p. 489 – 498;,
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. 268733-18-2, name is 4-Bromo-3,5-bis(trifluoromethyl)aniline, A new synthetic method of this compound is introduced below., Recommanded Product: 268733-18-2

General procedure: 4-Bromo-3,5-bis-(trifluoromethyl)aniline (616 mg, 2 mmol, 1 equiv), potassium carbonate (829 mg, 6 mmol, 3 equiv), Pd(PPh3)4 (231 mg, 0.2 mmol, 0.1 equiv), DMF (5 mL, 0.4 M) and (MeO)3B (0.28 mL, 2 mmol, 1 equiv) were added to a flask and the contents heated to 110 C overnight. The reaction solution was filtered using silica gel, Celite, and sea sand. The solvent was evaporated under reduced pressure and the residue was purified by column chromatography (1:5 EtOAc:Hex), to give 4-methyl-3,5-bis(trifluoromethyl)aniline (760 mg, 67%). 1H NMR (300 MHz, DMSO-d6): delta 2.42 (s, 3H), 3.88 (s, 2H), 7.09 (s, 2H). This aniline was used for general procedure A (EtOAc:Hex 1:20 ? 1:10) (630 mg, 51%). Slightly brown solid. Mp 192-193 C. 1H NMR (300 MHz, DMSO-d6): delta 2.49 (s, 3H), 7.02 (d, J = 8.8 Hz, 1H), 7.47 (dd, J1 = 8.8 Hz, J2 = 2.7 Hz, 1H), 7.87 (d, J = 2.6, 1H), 8.41 (s, 2H), 10.75 (s, 1H), 11.48 (s, br, 1H). HRMS (APCI), m/z calcd for C16H10ClF6NO2-H: 396.0226, found 396.0238.

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; Lee, Ill-Young; Gruber, Todd D.; Samuels, Amanda; Yun, Minhan; Nam, Bora; Kang, Minseo; Crowley, Kathryn; Winterroth, Benjamin; Boshoff, Helena I.; Barry III, Clifton E.; Bioorganic and Medicinal Chemistry; vol. 21; 1; (2013); p. 114 – 126;,
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. 10016-52-1, name is 2,8-Dibromodibenzo[b,d]furan, A new synthetic method of this compound is introduced below., HPLC of Formula: C12H6Br2O

To a round bottom flask triphenylen-2-ylboronic acid 8.4g, 2,8-dibromodibenzo[b,d]furan 10.0g dissolved in toluene 280 ml K2CO3(2M) 46 ml and Pd(PPh3)4 1.1g After putting the mixture was stirred under reflux. Check the reaction by TLC and the reaction was terminated after addition of water. After the organic layer was extracted with MC and the residue was filtered under reduced pressure, re-crystallized to give an intermediate I1-1 8.1g (56% yield).

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; Dongjin SemiChem Co. Pvt. Ltd.; Ham, Ho-Wan; Kim, Bong-Ki; Kim, Seong-Hun; Ahn, Hyun-Chul; Kim, Hee-Ju; Kim, Dong-Jun; Lee, Hyung-Jin; Lim, Dong-Hwan; Ahn, Ja-Eun; (42 pag.)KR2016/80090; (2016); A;,
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. 43204-63-3, name is Bis(2-Bromoethyl)amine hydrobromide, A new synthetic method of this compound is introduced below., category: bromides-buliding-blocks

REFERENCE EXAMPLE 6 A mixture of di(2-bromoethyl)amine hydrobromide (15.6 g; 0.05 mol), 3-aminobenzotrifluoride (24.2 g; 0.15 mol) and methylethylketone (50 ml) was heated under reflux for 4 hours, and the resultant mixture was neutralized with a dilute sodium hydroxide solution and extracted with ether. The ethereal layer was washed with a saturated sodium chloride solution and dried over anhydrous magnesium sulfate. The solvent was removed under reduced pressure, and the residue was distilled to give N-(alpha, alpha, alpha-trifluorom-tolyl)piperazine. B.P., 130-140 C./0.3 mmHg.

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; Sumitomo Chemical Company, Limited; US4598078; (1986); A;,
Bromide – Wikipedia,
bromide – Wiktionary

Electric Literature of 401-84-3, A common heterocyclic compound, 401-84-3, name is 1,3-Dibromo-5-(trifluoromethyl)benzene, molecular formula is C7H3Br2F3, 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.

Step 1 : 1-Bromo-3-(prop-1-en-2-yl)-5-(trifluoromethyl)benzene (P28a)To a solution of 1 ,3-dibromo-5-(trifluoromethyl)benzene (3.03 g, 10 mmol) in dioxane (20 mL) was added Pd(PPh3)4 (300 mg, 0.26 mmol), prop-1-en-2-ylboronic acid (1.0 g, 12 mmol), K2C03 (2.8 g, 20 mmol) and water (1 mL) under N2. The mixture was stirred at 90C overnight, concentrated and purified by CC (hexane) to afford compound P28a (1.9 g, 71%) as an oil.

The synthetic route of 401-84-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; PHENEX PHARMACEUTICALS AG; STEENECK, Christoph; KINZEL, Olaf; GEGE, Christian; KLEYMANN, Gerald; HOFFMANN, Thomas; WO2012/139775; (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. 955959-84-9, name is 4-(4-Bromophenyl)dibenzo[b,d]furan, A new synthetic method of this compound is introduced below., Application In Synthesis of 4-(4-Bromophenyl)dibenzo[b,d]furan

Preparation of compound C-6-2 [135] After dissolving compound C-6-1 (17 g, 52.6 mmol) in THF (400 ml), and adding 2.5 M n-BuLi in hexane (31.5 ml, 78.9 mmol) to the reaction mixture in -78°C, the reaction mixture was stirred for 1 hour. The reaction mixture was stirred for 12 hours with adding B(Oi-Pr) (24.1 ml, 105.2 mmol) slowly to the reaction mixture. After terminating the reaction, purified water 20 mL was dropped slowly to the reaction mixture. The reaction mixture was extracted with EA/NH4Cl aqueous solution. The obtained organic layer was concentrated, was triturated with MC/hexane, and then was filtered to obtain compound C-6-2 (14.5 g, 96 percent).

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; ROHM AND HAAS ELECTRONIC MATERIALS KOREA LTD.; AHN, Hee-choon; YOON, Seok-keun; KIM, Hee-sook; YANG, Soo-jin; LEE, Kyung-joo; KIM, Nam-kyun; CHO, Young-jun; KWON, Hyuck-joo; KIM, Bong-ok; WO2012/141499; (2012); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

These common heterocyclic compound, 955959-84-9, name is 4-(4-Bromophenyl)dibenzo[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. Computed Properties of C18H11BrO

250 ml of four-mouth bottle, in an atmosphere of nitrogen, adding 16.2 g 4 – (4 – bromo – phenyl) dibenzofuran (0.05 muM) and 1.44 gMg powder (0.06 muM), 60 ml tetrahydrofuran, heating reflux for 4 hours, the reaction is complete, generating format reagent; 11. 1g10, 10 – dimethyl anthrone (0.05 muM) dissolved in 50 ml in tetrahydrofuran, dropping the above-mentioned form reagent, 60 °C reaction 24 hours, generating a large amount of white precipitate, finally adding saturated NHCl4 The format salt into alcohol; after the reaction, diethyl ether extraction, drying and steaming and, petroleum ether: methylene chloride mixed solvent (3:2) silica gel column purification, to obtain slightly yellow solid tertiary alcohol (yield is 85percent);

The synthetic route of 4-(4-Bromophenyl)dibenzo[b,d]furan has been constantly updated, and we look forward to future research findings.

Reference:
Patent; CECEP Wanrun Co., Ltd.; Zhang Zhaochao; Wang Lichun; Li Chong; (29 pag.)CN107056737; (2017); A;,
Bromide – Wikipedia,
bromide – Wiktionary

These common heterocyclic compound, 626-39-1, name is 1,3,5-Tribromobenzene, 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. Formula: C6H3Br3

Under a nitrogen atmosphere, 250ml three-necked flask 1,3,5-bromobenzene (15.74g, 50mmol), United pinacolato ester (41.9g, 0.165mol, TCI), potassium acetate (48.58g, 0.495mol), 1,1′- bis (diphenylphosphino) ferrocene palladium dichloride (4.08g, 5mmol) and dimethylformamide (300ml), 85 The reaction mixture was stirred under heating 24h.After completion of the reaction naturally cooled, the reaction solution was extracted with ethyl acetate, washed with saturated brine three times, the resulting organic layer was dried over anhydrous magnesium sulfate.Filtration, the resulting filtrate was removed under reduced pressure to remove the solvent.Separated by column chromatography, the mobile phase was chloroform.After the spin-dry vacuum dried to give a white powder 16.25g, yield 71.3%.

The synthetic route of 1,3,5-Tribromobenzene has been constantly updated, and we look forward to future research findings.

Reference:
Patent; South China University of Technology; Su, Shijian; Chen, Dongcheng; (24 pag.)CN103396355; (2016); B;,
Bromide – Wikipedia,
bromide – Wiktionary

Reference of 43204-63-3, 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. 43204-63-3 name is Bis(2-Bromoethyl)amine hydrobromide, 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.

Formula X A mixture of 0.1 mol of bis-bromoethylamine hydrobromide and 0.1 mol of 2,4-difluoroaniline in 50 ml of butan-1-ol is heated at the boil for 14 hours. The reaction mixture is then cooled and the precipitate obtained is filtered off. The crystals are taken up with water and the mixture is rendered basic in the cold with a 10% solution of sodium hydroxide. The aqueous phase is extracted with chloroform and the extract is washed with water, dried over sodium carbonate and filtered. The chloroform is evaporated off and the residue obtained is taken up with acetone. Hydrogen chloride gas is bubbled through this solution, with stirring, until the pH is acid, and the crystals formed are allowed to settle. The crystals obtained are filtered off and then washed with acetone and dried. 4-(2,4-Difluorophenyl)piperazine dihydrochloride is thus recovered in the form of crystals melting at 205 C.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, Bis(2-Bromoethyl)amine hydrobromide, and friends who are interested can also refer to it.

Reference:
Patent; Centre D’Activite Et De Recherches Pharmaceutique Industrielle Biologique Medicale; US4886805; (1989); A;,
Bromide – Wikipedia,
bromide – Wiktionary