HRID2285663
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
31 g (0.2 mole) of 3,3-dimethyl-pent-4 -enoic acid, N,N-dimethylamide are added dropwise, in the course of 3 hours, to a solution of 1 g of azo-bis-isobutyronitrile in 308 g (2 moles) of carbon tetrachloride at 75°-80° C. The mixture is stirred for 1.5 hours at 75°-80° C., a further 1 g of azo-bis-isobutyronitrile is added, and the temperature is maintained for a further 2 hours. After distilling off the unconverted starting materials at a bath temperature not exceeding 150° C., a residue is left, and this is stirred with 100 ml of water at 80°-90° C. for 1 hour. 17 g (0.08 mole) of 5-(2,2-dichlorovinyl)-4,4-dimethyl-tetrahydrofuran-2-one are thereby obtained as a water-insoluble phase.
WORKUP
后处理
- temperaturethe temperature is maintained for a further 2 hours
- distillationAfter distilling off the
- customexceeding 150° C.
- waita residue is left
- stirringthis is stirred with 100 ml of water at 80°-90° C. for 1 hour