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
PROCEDURE
实验过程
235 g of 31% hydrochloric acid (2 moles) are metered into a mixture of 238 g of alpha-methyl styrene (2 moles) and 394 g of 80% tert.butyl hydroperoxide (3.5 moles) with stirring within 15 minutes, while the temperature of the mixture is allowed to rise from 20° C. to 35° C. Subsequently, stirring is continued for a further 2 hours at 40° C. then 250 ml water are added, the mixture is allowed to stand for 15 minutes and the aqueous phase is separated off. The organic phase is washed with 250 ml of 15% sodium hydroxide solution and twice with 500 ml of water in each case. After adding 20 g of water, the product is blown out with air at 50° C. (30 minutes). 395 g of a slightly yellowish liquid with a content of 96% tert.butyl cumyl peroxide and less than 0.4% alpha-methyl styrene are obtained. This corresponds to a yield of 91% based on the alpha-methyl styrene used.
WORKUP
后处理
- customto rise from 20° C. to 35° C
- stirringSubsequently, stirring
- waitis continued for a further 2 hours at 40° C.
- waitto stand for 15 minutes
- customthe aqueous phase is separated off
- washThe organic phase is washed with 250 ml of 15% sodium hydroxide solution and twice with 500 ml of water in each case
- additionAfter adding 20 g of water
- customis blown out with air at 50° C.
- custom(30 minutes)