HRID352111

反应详情

EQUATION

反应方程式

HRID 352111 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 1,1-dimethylethyl 4-oxo-4-phenylbutylcarbamate (2.4 g, 9.1 mmol), hydroxylamine hydrochloride (1.27 g, 2 equiv.) and sodium acetate trihydrate (2.5 g, 2 equiv.) was stirred and heated under reflux in 20% aqueous ethanol (60 ml) for 7 h. The reaction mixture was then concentrated and the residue partitioned between saturated aqueous sodium bicarbonate (100 ml) and ethyl acetate (200 ml). The organic extract was dried over magnesium sulphate and concentrated to afford a colourless solid (2.4 g, 95%).

WORKUP

后处理

  1. temperatureheated
  2. concentrationThe reaction mixture was then concentrated
  3. customthe residue partitioned between saturated aqueous sodium bicarbonate (100 ml) and ethyl acetate (200 ml)
  4. extractionThe organic extract
  5. dry with materialwas dried over magnesium sulphate
  6. concentrationconcentrated