反应详情

2,4-Difluoro-1-nitro-benzene (46, 1.4 mL, 13.0 mmol) and benzyl chloroformate (31, 10.42 g, 61.1 mmol) in 20 mL of tetrahydrofuran is cooled to −78° C. and stirred for 1 hour. Lithium diisopropylamine (1.5 g, 14.0 mmol) is added dropwise and the reaction is stirred at −78° C. for 1 hour, then warmed to room temperature over 2 hours. The reaction was purified by silica gel chromatography, eluting with hexane:ethyl acetate 90:10. Appropriate fractions are combined and concentrated under vacuum, then washed with methanol and the solid collected by filtration to provide the desired compound (47, 110 mg).

1. stirringthe reaction is stirred at −78° C. for 1 hour
2. customThe reaction was purified by silica gel chromatography
3. washeluting with hexane:ethyl acetate 90:10
4. concentrationconcentrated under vacuum
5. washwashed with methanol
6. filtrationthe solid collected by filtration