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ChemicalBook CAS DataBase List 2-Bromo-6-fluorobenzaldehyde
360575-28-6

2-Bromo-6-fluorobenzaldehyde synthesis

5synthesis methods
3-Bromofluorobenzene

1073-06-9

N,N-Dimethylformamide

68-12-2

2-Bromo-6-fluorobenzaldehyde

360575-28-6

To a stirred solution of iPr2NH (2.25 mL, 1.63 g, 16.1 mmol) in THF (20 mL) containing a 50 mL three-necked flask under the protection of dry argon gas was added dropwise nBuLi (6.3 mL, 2.35 M in hexane, 14.7 mmol). The reaction mixture was stirred at 0°C for 10 min. Subsequently, after continued stirring at 0°C for 20 min, the mixture was cooled to -78°C and a solution of 1-bromo-3-fluorobenzene (2.45 g, 14.0 mmol) in THF (10 mL) was added dropwise over a 12-minute period, maintaining the temperature in the range of -85 to -75°C, to give a deep red solution. After stirring at -78°C for 1 h, a THF (7 mL) solution of DMF (1.32 g, 18.2 mmol) was added dropwise over 5 min and stirring was continued for 1 h at -78°C. The reaction mixture was quenched with AcOH (2.5 mL) and slowly warmed to room temperature. The reaction mixture was poured into a mixture of 0.2 M HCl (40 mL) and MeOAc (50 mL) and the organic layer was separated. The aqueous layer was extracted with MeOAc (30 mL), and the combined organic phases were washed with brine (60 mL), dried over Na2SO4, filtered and concentrated under reduced pressure to give an orange colored oil. The oil was purified by recrystallization from hexane to afford the target product 2-bromo-6-fluorobenzaldehyde SI-1f (2.31 g, 11.4 mmol, 81% yield).

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Yield:360575-28-6 93%

Reaction Conditions:

Stage #1:3-fluorobromobenzene with n-butyllithium;N-ethyl-N,N-diisopropylamine in tetrahydrofuran;hexane at -78; for 1 h;Inert atmosphere;
Stage #2:Methyl formate in tetrahydrofuran;hexane at 20; for 0.5 h;Inert atmosphere;

Steps:

31.1 Step 1:
Step 1: (0458) Diisopropylamine (5.14 g, 50.8 mmol) was dissolved in dry tetrahydrofuran (50 ml) under a nitrogen atmosphere, n-butyllithium in hexane (20.3 ml, 50.8 mml) was added dropwise thereto at 0° C. followed by stirring for 30 minutes. The reaction mixture was cooled to -78° C., 1-bromo-3-fluorobenzene 31-a (10.0 g, 42.4 mml) in dry tetrahydrofuran (100 ml) solution was added dropwise thereto followed by stirring for 30 minutes. Methyl formate (7.63 g, 127.2 mml) was added dropwise thereto followed by stirring for 30 minutes. The mixture was warmed to room temperature, extracted with ethyl acetate (100 ml×3) and 1N hydrochloric acid (100 ml). The combined organic phase was dried over anhydrous sodium sulfate, filtered, concentrated, subjected to column chromatography to give 31-b as a white solid (8.0 g, yield: 93%).

References:

SHANGHAI INSTITUTE OF MATERIA MEDICA, CHINESE ACADEMY OF SCIENCES;SUZHOU VIGONVITA LIFE SCIENCES CO., LTD.;TOPHARMAN SHANDONG CO., LTD.;JIANG, Hualiang;WANG, Zhen;LI, Jianfeng;ZHANG, Rongxia;HE, Yang;LIU, Yongjian;BI, Minghao;LIU, Zheng;TIAN, Guanghui;CHEN, Weiming;YANG, Feipu;WU, Chunhui;WANG, Yu;JIANG, Xiangrui;YIN, Jingjing;WANG, Guan;SHEN, Jingshan US2017/158680, 2017, A1 Location in patent:Paragraph 0456; 0457; 0458

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