反应详情

The compound of example 95 (0.11 g) and copper(I) cyanide (0.03 g) were combined in N-methylpyrrolidinone (5 ml) and the mixture boiled for 6 h. After cooling to room temperature the reaction mixture was stood overnight, diluted with ethyl acetate, passed through silica gel eluting with ethyl acetate/water. The organic phase was separated washed with water dried (MgSO4) and solvent removed at reduced pressure. The residue was column chromatographed (silica gel, 20→100% ethyl acetate/pentane), the appropriate fractions combined and solvent removed at reduced pressure to give the title compound (0.03 g) as a gum

1. waitwas stood overnight
2. customThe organic phase was separated
3. washwashed with water
4. dry with materialdried (MgSO4) and solvent
5. customremoved at reduced pressure
6. customchromatographed (silica gel, 20→100% ethyl acetate/pentane)
7. customsolvent removed at reduced pressure