反应详情

460 mg of the aldehyde of example 5 in 8 ml of ether is mixed with 1.5 ml of a 3M methyl magnesium bromide solution in ether with ice cooling and is stirred for 20 hours at room temperature; 10 ml of tetrahydrofuran is added and heated to 60° C. in 6 hours. It is added to 1M of hydrochloric acid, extracted with ether, then the water phase is alkalized with potassium carbonate and extracted with ether. After drying and concentration by evaporation of this ether phase, the residue is chromatographed on silica gel (methylene chloride/methanol (95:5)). 300 mg of the title compound is obtained.

1. temperatureheated to 60° C. in 6 hours
2. extractionextracted with ether
3. extractionextracted with ether
4. customAfter drying
5. concentrationconcentration
6. customby evaporation of this ether phase
7. customthe residue is chromatographed on silica gel (methylene chloride/methanol (95:5))