反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- stirringafter stirring for 1 hour
- filtrationAfter filtration
- extractionthe filtrate was extracted with t-butyl methyl ether (300 ml) four times
- dry with materialThe organic layer put together was dried over magnesium sulfate
- filtrationsubjected to filtration
- distillationthe solvent was distilled off