反应详情

A solution of ethyl 2-{(5-methoxy-8-chlorosulfonyl -3,4-dihydro-4-oxospiro[2H-1-benzopyran-2,1'-cyclohexan]-7-yl)oxy}acetate (prepared in Preparation 70) (0.32 g, 0.74 mmol) in dichloromethane (4 ml) is added dropwise to a solution of liquid ammonia (2 ml, 80 mmol) and triethylamine (0.1 ml, 0.7 mmol) in dichloromethane (4 ml) at -25° to -20 ° C. After stirring at the same temperature for 30 minutes, the solvent is removed by distillation. The residue is placed on a silica gel column and eluted with a mixture of acetone and dichloromethane (1:1) to yield the title compound as a crystalline solid (0.173 g, yield 56.5%). Recrystallization from a mixture of ethyl acetate and ether gives a product having a melting point of 188°-190° C.

1. customthe solvent is removed by distillation
2. washeluted with a mixture of acetone and dichloromethane (1:1)