HRID2211203

反应详情

EQUATION

反应方程式

HRID 2211203 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of sodium azide (9.5 g, 0.14 mol), 3-bromomethyl-3-hydroxymethyloxetane (24.0 g, 0.14 mol), 20 mL of acetone and 20 mL of water was refluxed for 12 h. The acetone was evaporated and the resulting residue was extracted with two portion of 40 mL of ethyl acetate. The combined organic extracts were dried over magnesium sulfate (MgSO4). The solvent was removed by evaporation. 18.0 g, representing a 94% yield, of 3-azidomethyl-3-hydroxymethyloxetane were obtained as an oil. This oil was found to be essentially pure by gas-liquid chromatography (GLC) analysis. NMR: 1H NMR 3.70 (s, 2 H), 3.84 (d, J=4.9 Hz, 2 H), 4.44 (s, 4 H); 13C NMR 44.283, 53,852, 64,073, 76.227.

WORKUP

后处理

  1. temperaturewas refluxed for 12 h
  2. customThe acetone was evaporated
  3. extractionthe resulting residue was extracted with two portion of 40 mL of ethyl acetate
  4. dry with materialThe combined organic extracts were dried over magnesium sulfate (MgSO4)
  5. customThe solvent was removed by evaporation