HRID1369619

反应详情

EQUATION

反应方程式

HRID 1369619 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

A solution of Example 61A (254 mg, 0.793 mmol) in absolute ethanol (4 mL) was treated with anhydrous CaCl2 (177 mg, 1.59 mmol), stirred for 1 hour, cooled to 0° C., treated with NaBH4 (123 mg, 3.25 mmol), stirred at 0° C. for 4 hours and at room temperature for 18 hours, treated with water and extracted with dichloromethane. The extract was washed with brine, dried (Na2SO4), filtered and concentrated. The residue was purified on silica gel with 30% ethyl acetate/hexane to provided the title compound.

WORKUP

后处理

  1. stirringstirred at 0° C. for 4 hours and at room temperature for 18 hours
  2. extractionextracted with dichloromethane
  3. washThe extract was washed with brine
  4. dry with materialdried (Na2SO4)
  5. filtrationfiltered
  6. concentrationconcentrated
  7. customThe residue was purified on silica gel with 30% ethyl acetate/hexane