HRID1909088

反应详情

EQUATION

反应方程式

HRID 1909088 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of β-methallyl alcohol (10 g, 139 mmol) and sodium tungstate dihydrate (92 mg, 0.28 mmol) was stirred at room temperature, and a 35% hydrogen peroxide solution (17.3 g, 153 mmol) was added thereto dropwise over a period of 5 minutes. The mixture was heated to 40° C. and stirred for 7 hours. Potassium carbonate (9.6 g, 69 mmol) and 4-bromophenol (7.9 g, 46 mmol) were added to a half amount of the resulting reaction mixture (70 mmol, based on β-methallyl alcohol), followed by stirring at 60° C. for 2.5 hours. After adding toluene (30 ml), the mixture was heated, washed with water at a temperature about 60° C., and then cooled with ice. The precipitated crystals were collected by filtration, washed with toluene (5 ml), and then dried under reduced pressure, obtaining 9.8 g of 3-(4-bromophenoxy)-2-methylpropane-1,2-diol (yield: 82% (based on 4-bromophenol)).

WORKUP

后处理

  1. temperatureThe mixture was heated to 40° C.
  2. stirringstirred for 7 hours
  3. stirringby stirring at 60° C. for 2.5 hours
  4. temperaturethe mixture was heated
  5. washwashed with water at a temperature about 60° C.
  6. temperaturecooled with ice
  7. filtrationThe precipitated crystals were collected by filtration
  8. washwashed with toluene (5 ml)
  9. customdried under reduced pressure