HRID1044050
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- stirringThe mixture was stirred at 0° C. for 10 minutes
- stirringstirred for additional 30 minutes
- concentrationThe reaction mixture was concentrated under vacuum
- customthe residue was partitioned between Et2O and ice-
- temperaturecooled water
- customThe organic layer was separated
- washwashed with water and brine
- dry with materialdried over Na2SO4
- filtrationfiltered
- customevaporated (5.05 g, 91% yield)