HRID1044050

反应详情

EQUATION

反应方程式

HRID 1044050 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of ethyl 2-oxo-2-(thiophen-2-yl)acetate (5.00 g, 27.1 mmol) in ethanol (50 ml) was cooled at 0° C. with an ice bath. NaBH4 (0.31 g, 8.14 mmol) was added in four portions under stirring. The mixture was stirred at 0° C. for 10 minutes, then allowed to warm at room temperature and stirred for additional 30 minutes. The reaction mixture was concentrated under vacuum and the residue was partitioned between Et2O and ice-cooled water. The organic layer was separated, washed with water and brine, dried over Na2SO4, filtered and evaporated (5.05 g, 91% yield).

WORKUP

后处理

  1. stirringThe mixture was stirred at 0° C. for 10 minutes
  2. stirringstirred for additional 30 minutes
  3. concentrationThe reaction mixture was concentrated under vacuum
  4. customthe residue was partitioned between Et2O and ice-
  5. temperaturecooled water
  6. customThe organic layer was separated
  7. washwashed with water and brine
  8. dry with materialdried over Na2SO4
  9. filtrationfiltered
  10. customevaporated (5.05 g, 91% yield)