反应详情

Diisobutylaluminum hydride (0.236 mol, 236 mL of a 1 M solution in hexane) is added over 90 minutes to a solution of p-chloro-α-methylhydratroponitrile (32.6 g, 0.181 mol) in diethyl ether under nitrogen at 0° C. After the addition is complete, water and 6 N hydrochloric acid are added to the reaction mixture while maintaining the temperature below 30° C. The resultant aqueous solution is stirred overnight at room temperature and extracted with diethyl ether. The organic extracts are combined, washed sequentially with 2 N hydrochloric acid and water, dried over anhydrous sodium sulfate, and concentrated in vacuo to give the title product as an oil (31.1 g, 94% yield).

1. additionAfter the addition
2. temperaturewhile maintaining the temperature below 30° C
3. extractionextracted with diethyl ether
4. washwashed sequentially with 2 N hydrochloric acid and water
5. dry with materialdried over anhydrous sodium sulfate
6. concentrationconcentrated in vacuo