HRID344047

反应详情

EQUATION

反应方程式

HRID 344047 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of 5-t-butyldiphenylsilyloxy-2-ethoxycarbonyl-1-oxo-1,2,3,4-tetrahydronaphthalene (17 g) in a mixture of ethanol (100 ml) and tetrahydrofuran (100 ml) was added NaBH4 (1.4 g) at 0° C. After the mixture was stirred for 6 hours at room temperature, the solvent was removed in vacuo. The residue was dissolved in a mixture of ethyl acetate and water and the organic solution was washed with 1N-HCl solution, sat. NaHCO3, and brine. The dried solvent was evaporated in vacuo and the residue was purified by chromatography on silica gel to give 1-hydroxy-2-ethoxycarbonyl-5-t-butyldiphenylsilyloxy-1,2,3,4-tetrahydronaphthalene (7.9 g).

WORKUP

后处理

  1. customthe solvent was removed in vacuo
  2. dissolutionThe residue was dissolved in a mixture of ethyl acetate and water
  3. washthe organic solution was washed with 1N-HCl solution, sat. NaHCO3, and brine
  4. customThe dried solvent was evaporated in vacuo
  5. customthe residue was purified by chromatography on silica gel