HRID748075

反应详情

EQUATION

反应方程式

HRID 748075 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a stirred mixture of 1-[1-(benzyloxy)-1H-pyrazol-5-yl]-2-ethylbutan-1-ol (0.492 g, 1.79 mmol) in THF (17 mL) at 0° C. under a nitrogen atmosphere was added triphenyl phosphine (0.705 g, 2.69 mmol) followed by diethyl azodicarboxylate (0.42 mL, 2.7 mmol). Diphenyl phosphoryl azide (0.58 mL, 2.7 mmol) was then added over 4 min. The mixture was allowed to attain ambient temperature and stirred for 16 h. The solvent was then evaporated in vacuo producing a crude oil which was purified on a Biotage column (hexane/ethyl acetate, 9:1). This afforded the product as a clear colorless oil (0.36 g, 67%). Mass Spectrum (+ESI): 300 (M+H)+.

WORKUP

后处理

  1. customto attain ambient temperature
  2. customThe solvent was then evaporated in vacuo
  3. customproducing a crude oil which
  4. customwas purified on a Biotage column (hexane/ethyl acetate, 9:1)