HRID1666702

反应详情

EQUATION

反应方程式

HRID 1666702 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

0.73 g (7 mmol) ethyl hydroxyacetate is dissolved in 20 ml tetrahydrofurane and 0.36 g (9 mmol) 60% sodium hydride is added to it. After 20 minute stirring 1.0 g (6 mmol) 2-chloro-6-methyl-1,3-benzoxazole is added and the mixture is heated under reflux for 3 hours. The solvent is removed, the residue is dissolved in 15 ml water, extracted with 3×20 ml ethyl acetate. The united organic phase is dried over sodium sulfate and evaporated to obtain 1.3 g title compound as an oil. LC-MS[MH+]=236 (C12H13NO4 235.24)

WORKUP

后处理

  1. additionis added
  2. temperaturethe mixture is heated
  3. temperatureunder reflux for 3 hours
  4. customThe solvent is removed
  5. dissolutionthe residue is dissolved in 15 ml water
  6. extractionextracted with 3×20 ml ethyl acetate
  7. dry with materialThe united organic phase is dried over sodium sulfate
  8. customevaporated