HRID446507

反应详情

EQUATION

反应方程式

HRID 446507 的结构方程式

PROCEDURE

实验过程

The compound (449 mg, 1.16 mmol) obtained in Example 5b was dissolved in tert-butanol (6 mL), triethylamine (1.78 mL, 1.28 mmol) and diphenylphosphate azide (0.251 mL, 1.16 mmol) were added, and the mixture was stirred with heating to reflux for 3 hours. The solvent was evaporated under reduced pressure, and the resulting residue was purified by silica gel column chromatography (hexane:ethyl acetate=1:2→0:100, v/v) to give the title compound (339 mg; yield, 64%) as a colorless oily substance.

WORKUP

后处理

  1. temperaturewith heating
  2. temperatureto reflux for 3 hours
  3. customThe solvent was evaporated under reduced pressure
  4. customthe resulting residue was purified by silica gel column chromatography (hexane:ethyl acetate=1:2→0:100, v/v)