反应详情

To a mixture of 19.3 g. of methylene bromide and 3.7 g. of triethylamine in 100 ml. of dimethylformamide was added 10.0 g. of potassium p-chlorophenoxymethyldithiocarbamate in portions. After one to two hours, the mixture was poured into water and partitioned into ethylene chloride. The dried ethylene chloride mixture was saturated with dry hydrogen chloride and the resulting salt collected by filtration. Hydrolysis of the salt in a chloroform-water mixture followed by separation, drying and concentration of the chloroform layer gave 3.5 g. of the dithietane as pale yellow crystals, m.p. 64.5°-66.0° C.

1. additionTo a mixture of 19.3 g
2. waitAfter one to two hours
3. custompartitioned into ethylene chloride
4. filtrationthe resulting salt collected by filtration
5. customHydrolysis of the salt in a chloroform-water mixture
6. customfollowed by separation
7. customdrying
8. customconcentration of the chloroform layer gave 3.5 g