HRID1713045

反应详情

EQUATION

反应方程式

HRID 1713045 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Sodium azide (76 mg, 1.17 mmol) and triethylamine hydrochloride (161 mg, 1.17 mmol) are added to a solution of Compound 35 (462.5 mg, 1.25 mmol) dissolved in DME (15 ml) and the suspension is refluxed for 48 hours. The mixture is then cooled to room temperature and the solvent is removed under reduced pressure. Water (30 ml) and ethyl acetate (30 ml) are added thereto and the aqueous phase is extracted three more times with ethyl acetate. The combined organic extracts are dried over Na2SO4 and the solvent is evaporated under reduced pressure. The crude product is recrystallized from ethanol to give Compound 36.

WORKUP

后处理

  1. temperaturethe suspension is refluxed for 48 hours
  2. customthe solvent is removed under reduced pressure
  3. additionWater (30 ml) and ethyl acetate (30 ml) are added
  4. extractionthe aqueous phase is extracted three more times with ethyl acetate
  5. dry with materialThe combined organic extracts are dried over Na2SO4
  6. customthe solvent is evaporated under reduced pressure
  7. customThe crude product is recrystallized from ethanol