反应详情

The silyl cyanohydrin of Example 3 (40.7 g, 165 mol) was dissolved in 300 ml ethanol and perfused at 0° C. with hydrogen chloride for 30 minutes. After an additional 16 hours at 0° C. the mixture was evaporated in vacuo to an oil. This was taken up in chloroform and washed with 2×100 ml sodium bicarbonate, 1×80 ml water, 1×80 ml brine, dried over magnesium sulfate, filtered, and evaporated in vacuo to a residue which partially crystallized. This solid was triturated with 10% ethereal hexane 17.6 g (62%) mp 55°-59° C. (69°-75° C. after recrystallization from ether/hexane).

1. customAfter an additional 16 hours at 0° C. the mixture was evaporated in vacuo to an oil
2. washwashed with 2×100 ml sodium bicarbonate, 1×80 ml water, 1×80 ml brine
3. dry with materialdried over magnesium sulfate
4. filtrationfiltered
5. customevaporated in vacuo to a residue which
6. custompartially crystallized
7. customThis solid was triturated with 10% ethereal hexane 17.6 g (62%) mp 55°-59° C. (69°-75° C. after recrystallization from ether/hexane)