HRID1264624

反应详情

EQUATION

反应方程式

HRID 1264624 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Methyl 3-amino-4-hydroxyphenylacetate (5.43 g, 0.03 mol) was suspended in toluene (60 ml) and 1,1′-thiocarbonyldiimidazole (5.34 g, 0.03 mol) was added. The resultant mixture was stirred for 30 minutes, then acetic acid (10 ml) was added and the mixture was heated under reflux for 3 hours. The mixture was cooled to room temperature and the solvent was removed in vacuo. The residue was partitioned between water and ethyl acetate The organic extract was dried over magnesium sulfate, filtered and the filtrate was evaporated to give methyl (2,3-dihydro-2-thioxo-5-benzoxazolyl)acetate (6,2 g) as a light brown solid, m.p. 120-122° C.

WORKUP

后处理

  1. temperaturethe mixture was heated
  2. temperatureunder reflux for 3 hours
  3. customthe solvent was removed in vacuo
  4. customThe residue was partitioned between water and ethyl acetate The
  5. extractionorganic extract
  6. dry with materialwas dried over magnesium sulfate
  7. filtrationfiltered
  8. customthe filtrate was evaporated