反应详情

A solution of 2-amino-4-(4-chloro-phenyl)-butyronitril (0.425 g, 2.18 mmol) in tetrahydrofurane (4 ml) was added dropwise to a suspension of lithium aluminum hydride (0.331 g, 8.73 mmol) in tetrahydrofurane (4 ml) at 0° C. under argon atmosphere. The reaction mixture was allowed to reflux overnight. After cooling to 0° C. solid sodium sulphate decahydrate was added and stirring was continued for 1 hour. The grey suspension was filtered through Celite and the solvent was evaporated. The residue was purified by chromatography (column: Isolute® Flash-NH2 from Separtis; eluent:ethyl acetate/methanol=90:10) to yield a colorless oil (0.091 g, 21%); MS (ISP): 199.1 ((M+H)+).

1. temperatureto reflux overnight
2. additionwas added
3. filtrationThe grey suspension was filtered through Celite
4. customthe solvent was evaporated
5. customThe residue was purified by chromatography (column: Isolute® Flash-NH2 from Separtis; eluent:ethyl acetate/methanol=90:10)