反应 #4243

ord-2a2a0d78cbcc499984b40bbe74b117a2

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他equipped with thermometer, stirrer, cooler and drip funnel
  2. 2
    其他is held at this temperature overnight
  3. 3
    洗涤the resultant solution is washed twice with 3% NaOH solution until neutral,
  4. 4
    干燥dried over sodium sulfate
  5. 5
    过滤filtered
  6. 6
    浓缩The filtrate is concentrated

实验过程

A 350 ml sulfurating flask equipped with thermometer, stirrer, cooler and drip funnel is charged with 21.8 g (0.10 mole) of 4-allyl-2,6-dimethylphenyl glycidyl ether, 10.9 g (0.24 mole) of formic acid and 135 ml of chloroform. At room temperature, 23.2 g (0.47 mole) of hydrogen peroxide are then added dropise over 4 hours. The reaction miture is held at this temperature overnight. It is subsequently taken up in chloroform and the resultant solution is washed twice with 3% NaOH solution until neutral, made peroxide-free with sodium sulfite, dried over sodium sulfate and filtered. The filtrate is concentrated, affording 20.03 g (80.50% of theory) of 4-(2,3-epoxypropyl)-2,6-dimethylphenyl glycidyl ether in the form of a low viscous resin; epoxide content 7.7 equivalents/kg (90.11% of theory).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US04724031uspto-grants-1988_02