反应详情

A mixture of 300 mg of the aldehyde (prepared as described in Reference Example 1), 370 mg of sodium cyanide, 3.0 g of manganese dioxide, 0.18 ml of acetic acid and 15 ml of methanol was stirred overnight at room temperature, filtered through a pad of infusorial earth, and the filtrate was concentrated under reduced pressure. To the residue was added a saturated aqueous solution of sodium bicarbonate, and extracted with chloroform. The extract was washed with water, 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 (3:2) as eluent to give 255 mg of the title compound having the following physical characteristics:

1. filtrationfiltered through a pad of infusorial earth
2. concentrationthe filtrate was concentrated under reduced pressure
3. additionTo the residue was added a saturated aqueous solution of sodium bicarbonate
4. extractionextracted with chloroform
5. washThe extract was washed with water
6. dry with materialdried over sodium sulphate
7. concentrationconcentrated under reduced pressure
8. customThe residue was purified by column chromatography on silica gel using
9. additiona mixture of cyclohexane and ethyl acetate (3:2) as eluent