HRID748031

反应详情

EQUATION

反应方程式

HRID 748031 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

38 g of 4,5-Dimethyl-2-(4-(2-propyl)-phenyl)-oxazole 3-oxide are dissolved in 200 ml of chloroform, 16.4 ml of phosphorus oxychloride are added and the mixture is heated under reflux for 30 minutes. The reaction mixture is cooled to 0° C., a slightly alkaline pH is established using ammonia and the mixture is extracted three times with in each case 500 ml of ethyl acetate. The combined organic phases are washed with water and dried over MgSO4 and the solvent is then removed under reduced pressure. The residue is purified on silica gel using the mobile phase n-heptane:ethyl acetate=80:1=>5:1. This gives 10.3 g of 4-chloromethyl-5-methyl-2-(4-(2-propyl)-phenyl)-oxazole as a colorless solid. C14H16CINO (249.74), MS(ESI): 250 (M+H+).

WORKUP

后处理

  1. temperaturethe mixture is heated
  2. temperatureunder reflux for 30 minutes
  3. extractionthe mixture is extracted three times with in each case 500 ml of ethyl acetate
  4. washThe combined organic phases are washed with water
  5. dry with materialdried over MgSO4
  6. customthe solvent is then removed under reduced pressure
  7. customThe residue is purified on silica gel using the mobile phase n-heptane