反应详情

A solution of (E)- and/or (Z)-N-hydroxy-2-fluoro-benzenecarboximidoyl chloride (6.5 g, 37 mmol) in ethanol (29 mL) was added dropwise to a solution of acetylacetone (4.6 g, 46 mmol) containing sodium ethoxide (14.8 g, 46 mmol) in ethanol (83 mL) at ice-bath cooling temperature. After complete addition, the resulting mixture was allowed to warm up to room temperature and stirred for 1.5 h. The mixture was then acidified with HCl (6 N) and concentrated and the mixture extracted with ethyl acetate and then washed with water and brine and dried over sodium sulphate. Purification by chromatography (SiO2, heptane:ethyl acetate=100:0 to 75:25) afforded the title compound (7.0 g, 85%) which was obtained as a light yellow liquid. MS: m/e=220.1 [M+H]+.

1. temperaturecooling temperature
2. additionAfter complete addition
3. concentrationconcentrated
4. extractionthe mixture extracted with ethyl acetate
5. washwashed with water and brine
6. dry with materialdried over sodium sulphate
7. customPurification by chromatography (SiO2, heptane:ethyl acetate=100:0 to 75:25)