HRID2236537

反应详情

EQUATION

反应方程式

HRID 2236537 的结构方程式

CONDITIONS

反应条件

温度
90 °C

PROCEDURE

实验过程

A mixture of 2-hydroxymethyl-5-propoxy-pyran-4-one (30.0 g, 0.163 mole), 150 mL ammonium hydroxide is stirred and heated in a sealed vessel at 90° C. for 2 hours. The reaction mixture is cooled, evaporated to dryness in-vacuo, taken up in 15% methanol in chloroform and passed thru a pad of magnesol and silica gel eluting with the same solvent. The eluate is evaporated, treated with acetone, filtered, washed with acetone and air dried to give a-grey solid, 8.03 g, (80%), m.p. 159-60° C.; MS (ES+): m/z 184.3 (M+H).

WORKUP

后处理

  1. temperatureThe reaction mixture is cooled
  2. customevaporated to dryness in-vacuo
  3. customThe eluate is evaporated
  4. additiontreated with acetone
  5. filtrationfiltered
  6. washwashed with acetone and air
  7. customdried
  8. customto give a-grey solid, 8.03 g, (80%), m.p. 159-60° C.