反应详情

Under an atomsphere of nitrogen, 1.5 ml of a 3M solution of methylmagnesium iodide in diethyl ether were added to a solution of 830 mg of the aldehyde(prepared as described in Reference Example 1) in 20 ml of tetrahydrofuran at -70° C., the mixture was allowed to warm from -70° C. to room temperature over a period of one hour with stirring, poured into a saturated aqueous solution of ammonium chloride, and extracted with diethyl ether. The extract was washed with water, and a saturated aqueous solution of sodium chloride, dried over sodium sulphate and concentrated under reduced pressure. The residue was purified by column chromatography on silica gel using a mixture of cyclohexane and ethyl acetate (1:1) as eluent to give 547 mg of the title compound having the following physical characteristics:

1. temperatureto warm from -70° C. to room temperature over a period of one hour
2. extractionextracted with diethyl ether
3. washThe extract was washed with water
4. dry with materiala saturated aqueous solution of sodium chloride, dried over sodium sulphate
5. concentrationconcentrated under reduced pressure
6. customThe residue was purified by column chromatography on silica gel using
7. additiona mixture of cyclohexane and ethyl acetate (1:1) as eluent