Dimethylformamide → 4-Bromo-2,5-difluorobenzaldehyde

温度

-78 °C

n-Butyl lithium (3.6 ml, 7.7 mmol) was added drop wise to a solution of 1,4-dibromo-2,5-difluoro-benzene (2 g, 7.35 mmol) in dry ether at −78° C. under nitrogen atmosphere and the resulting mixture was stirred at −78° C. for 30 minutes. This was followed by the addition of DMF (0.85 ml, 11.03 mmol) in dry THF. The resultant was stirred at room temperature for 1 hour. The reaction was monitored by TLC (5% ethyl acetate in hexane). The reaction mixture was partitioned between ethyl acetate and saturated ammonium chloride. The organic layer was concentrated and purified by column chromatography on silica gel (2% ethyl acetate in hexane) to afford 600 mg of the product (37% yield).

1. stirringThe resultant was stirred at room temperature for 1 hour
2. customThe reaction mixture was partitioned between ethyl acetate and saturated ammonium chloride
3. concentrationThe organic layer was concentrated
4. custompurified by column chromatography on silica gel (2% ethyl acetate in hexane)

ORDレコード

ord-7cd451ad649e4ed0b5e0aa8c26055201

出典データセット

uspto-grants-2016_05

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US09339501B2