HRID1155964

反应详情

EQUATION

反应方程式

HRID 1155964 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

5-Cyano-2,3-dihydro-3,3-dimethyl-2-hydroxybenzofuran (2.0 g), prepared as in Example 10, was dissolved in methanol (10 ml) and added to sodium hydroxide (1.7 g) in water (25 ml) at 10°-15° C. with stirring. To this solution was added sodium borohydride (0.5 g), and the mixture was stirred at ambient temperature for 11/2 hours. After acidification with hydrochloric acid (6 ml) at 8°-12° C., the mixture was filtered and the product washed with water and dried yielding 1.8 g. Recrystallisation from toluene gave 1.2 g of product, mp 129°-130° C.

WORKUP

后处理

  1. stirringthe mixture was stirred at ambient temperature for 11/2 hours
  2. filtrationAfter acidification with hydrochloric acid (6 ml) at 8°-12° C., the mixture was filtered
  3. washthe product washed with water
  4. customdried
  5. customyielding 1.8 g
  6. customRecrystallisation from toluene