反应详情

Thionyl chloride (4.2 g) in diethyl ether (10 ml) was added dropwise with stirring at 0°-5° C. to a solution of 2-(5-cyano-2-hydroxyphenyl)-2-methyl-1-propanol (5 g) prepared as in Example 26, and pyridine (5.5 g) in diethyl ether (80 ml). The mixture was stirred for 3 hours at 0°-20° C. Water was then added and the mixture was filtered. The ether solution was then washed with dilute hydrochloric acid, when with aqueous sodium bicarbonate and water (twice), then dried over magnesium sulphate and run down. The residue was recrystallised from ethanol, giving the title product (2.0 g) as white crystals, mp 87°-88° C.

1. filtrationthe mixture was filtered
2. washThe ether solution was then washed with dilute hydrochloric acid, when with aqueous sodium bicarbonate and water (twice),
3. dry with materialthen dried over magnesium sulphate
4. customThe residue was recrystallised from ethanol