反应详情

Approximately 50 ml. of liquid ammonia is condensed in a three-neck flask cooled to -78° in a dry ice-acetone bath. To this is added 200 mg. of sodium metal, followed by 100 mg. of ferric chloride hexahydrate. When the blue color had vanished, 6.2 g. of 2-(p-fluorobenzoyl)-3-methoxycrotononitrile is added. After stirring for one hour, the reaction is allowed to warm and the solvent evaporate. The residue is dissolved in hot ethyl acetate and filtered through Celite®. The filtrate is concentrated on the steam bath and diluted with hexane. Upon cooling, the crystalline product precipitates, is filtered and dried.

1. customcondensed in a three-neck flask
2. temperaturecooled to -78° in a dry ice-acetone bath
3. additionTo this is added 200 mg
4. temperatureto warm
5. customthe solvent evaporate
6. dissolutionThe residue is dissolved in hot ethyl acetate
7. filtrationfiltered through Celite®
8. concentrationThe filtrate is concentrated on the steam bath
9. additiondiluted with hexane
10. temperatureUpon cooling
11. customthe crystalline product precipitates
12. filtrationis filtered
13. customdried