反应详情

4.3 gm=3.9 ml (0.025 mol) of benzyl chloroformate dissolved in 15 ml of methylene chloride, were added dropwise to a solution of 4.9 gm (0.02 mol) of 1-benzyl-4-chloro-5-cyano-2,3,6,7-tetrahydro-1H-azepine in 500 ml of methylene chloride while stirring at room temperature, whereby the temperature rose by 5° C. The mixture was stirred for 5 hours at room temperature and then allowed to stand overnight. The solvent was then removed in a rotary evaporator, and the residue was purified on a silicagel column (toluene/ethyl acetate=8:2). After the corresponding fractions had been concentrated by evaporation, a slightly yellowish oil was obtained with solidified upon standing.

1. customrose by 5° C
2. stirringThe mixture was stirred for 5 hours at room temperature
3. customThe solvent was then removed in a rotary evaporator
4. customthe residue was purified on a silicagel column (toluene/ethyl acetate=8:2)
5. concentrationAfter the corresponding fractions had been concentrated by evaporation
6. customa slightly yellowish oil was obtained with solidified