反应详情

To 12.7 g of 4-chloro-5-difluoromethoxy-2-fluorophenylhydrazine were added 127 ml of toluene and 9.5 g of 2-ethoxycarbonylcyclohexanone V-1, and the resultant mixture was refluxed for 24 hours. After cooling, the reaction mixture was mixed with water and shaken with chloroform. The chloroform layer was dried and concentrated. The residue was chromatographed on a column of silica gel, eluting with n-hexane-ethyl acetate (1:1 v/v). The elutate was concentrated to give 6,0 g of the titled compound VIII-1 (containing a certain amount of its tautomer 2,3a,4,5,6,7-hexahydro compound).

1. temperatureAfter cooling
2. dry with materialThe chloroform layer was dried
3. concentrationconcentrated
4. customThe residue was chromatographed on a column of silica gel
5. washeluting with n-hexane-ethyl acetate (1:1 v/v)
6. concentrationThe elutate was concentrated