HRID980303

反应详情

EQUATION

反应方程式

HRID 980303 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of N-(methylsulphonyl)acetamide potassium salt (23 g) and 4-nitrobenzyl bromide (24 g) in dry DMF (160 ml) was stirred in an oil bath at 130° for 2 h. After standing overnight at room temperature, a solution of sodium hydroxide (8 g) in water (50 ml) was added and the mixture stirred under nitrogen for 0.75 h. The mixture was diluted with water (900 ml) and the product extracted into ethyl acetate (2×400 ml). The combined extract was washed with brine (3×200 ml), dried (Na2SO4) and evaporated in vacuo to leave an orange solid (22 g).

WORKUP

后处理

  1. waitAfter standing overnight at room temperature
  2. stirringthe mixture stirred under nitrogen for 0.75 h
  3. extractionthe product extracted into ethyl acetate (2×400 ml)
  4. extractionThe combined extract
  5. washwas washed with brine (3×200 ml)
  6. dry with materialdried (Na2SO4)
  7. customevaporated in vacuo