HRID252248

反应详情

EQUATION

反应方程式

HRID 252248 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
4 °C

PROCEDURE

实验过程

To a chilled solution (ice-bath) of 4-methyl-5-phenyl-oxazole (0.2 g, 1.3 mmol) in CHCl3 (1 ml) was added drop-wise chlorosulfonic acid (0.5 ml, 7.7 mmol). The dark-brown reaction mixture was stirred at 4° C. for 30 min and slowly warmed to reflux. After 2 h the reaction mixture was poured into ice-water and extracted with ethyl acetate (3×). The combined organic extracts were washed with water, brine, dried (MgSO4.2H2O), filtered and evaporated to yield a light-brown solid: 0.19 g, (56%), MS: m/e 257.1.

WORKUP

后处理

  1. temperatureslowly warmed to reflux
  2. extractionextracted with ethyl acetate (3×)
  3. washThe combined organic extracts were washed with water, brine
  4. dry with materialdried (MgSO4.2H2O)
  5. filtrationfiltered
  6. customevaporated
  7. customto yield a light-brown solid