HRID2308043

反应详情

EQUATION

反应方程式

HRID 2308043 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
75 °C

PROCEDURE

实验过程

Into a reactor, 1,3-propanediol (46.7 g) and potassium hydroxide (34.5 g) were charged and stirred, and heated at the internal temperature of 75° C. for 30 minutes. At the internal temperature of 80° C., CH2═CH(CH2)2OTs (69.5 g) obtained in EXAMPLE 3-1 was added thereto over 3 hours and standed as it is after stirring for 1 hour. The reaction mixture was poured into water (250 ml) and neutralized by adding hydrochloric acid. After filtration, the filtrate was extracted with t-butyl methyl ether (300 ml) four times. The organic layer put together was dried over magnesium sulfate and subjected to filtration, and the solvent was distilled off to obtain 5.5 g of CH2═CH(CH2)2O(CH2)3OH.

WORKUP

后处理

  1. stirringafter stirring for 1 hour
  2. filtrationAfter filtration
  3. extractionthe filtrate was extracted with t-butyl methyl ether (300 ml) four times
  4. dry with materialThe organic layer put together was dried over magnesium sulfate
  5. filtrationsubjected to filtration
  6. distillationthe solvent was distilled off