반응 #2060760

반응 방정식

dithietane

methylene bromide

triethylamine

potassium p-chlorophenoxymethyldithiocarbamate

→

2-(p-Chlorophenoxymethylimino)-1,3-dithietane

용매

dimethylformamide

water

반응 조건

후처리

1. 1
   workup.ADDITIONTo a mixture of 19.3 g
2. 2
   workup.WAITAfter another one to two hours
3. 3
   기타partitioned into ethylene chloride
4. 4
   여과the resulting salt collected by filtration
5. 5
   기타Hydrolysis of the salt in a chloroform-water mixture
6. 6
   기타followed by separation
7. 7
   기타drying
8. 8
   기타concentration of the chloroform layer gave 3.5 g

실험 절차

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 another 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.

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