HRID1807533

反应详情

EQUATION

反应方程式

HRID 1807533 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

To a stirred solution of 3-hydroxy-5-methylisoxazole (5.0 g, 50.5 mmol) in acetone (125 mL) at room temperature under argon was added K2CO3 (13.9 g, 101 mmol) and the reaction mixture was heated at 60° C. After 30 min, 1-bromo-2-methylpropane (10.4 g, 75.7 mmol) was added dropwise over 2 min. After 16 h the reaction mixture was cooled, filtered and concentrated. Purification by chromatography (silica, 70 to 100% ethyl acetate in heptane) gave the title compound (700 mg, 9%) as a volatile yellow liquid.

WORKUP

后处理

  1. temperatureAfter 16 h the reaction mixture was cooled
  2. filtrationfiltered
  3. concentrationconcentrated
  4. customPurification by chromatography (silica, 70 to 100% ethyl acetate in heptane)