反应详情

Thionyl chloride (9.3 g) in dichloromethane (10 ml) was added dropwise with stirring and cooling to 5-cyano-2,3-dihydro-3,3-dimethyl-2-hydroxybenzofuran (11.3 g) prepared as in Example 10 and pyridine (6.2 g) in dichloromethane (60 ml). The mixture was stirred for 2 hours at room temperature prior to washing with water, dilute sodium hydroxide solution and water again, drying over magnesium sulphate and evaporating under vacuum. Recrystallisation from toluene and petroleum ether (bp 80°-100° C.) gave 9.7 g of the title compound, mp 105°-106° C.

1. stirringThe mixture was stirred for 2 hours at room temperature
2. washto washing with water, dilute sodium hydroxide solution and water again
3. dry with materialdrying over magnesium sulphate
4. customevaporating under vacuum
5. customRecrystallisation from toluene and petroleum ether (bp 80°-100° C.)