HRID45188

反应详情

EQUATION

反应方程式

HRID 45188 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2.91 g of [1-Methyl-1-(4-oxo-cyclohexyl)-ethyl]-carbamic acid tert-butyl ester (20) were dissolved in 60 mL of ethanol and 473 mg of sodium borohydride were added at −20° C. The mixture was allowed to warm to room temperature and stirred for 3.5 h. The mixture was evaporated, the residue was dissolved in ethyl acetate and washed twice with 2N hydrochloric acid and once with brine. The organic layer was dried over sodium sulphate and evaporated to dryness to give 2.74 g of (21). Rt=1.27 min (Method 5). Detected mass: 194 (M-Isobutene-H2O+H+).

WORKUP

后处理

  1. customThe mixture was evaporated
  2. dissolutionthe residue was dissolved in ethyl acetate
  3. washwashed twice with 2N hydrochloric acid and once with brine
  4. dry with materialThe organic layer was dried over sodium sulphate
  5. customevaporated to dryness