반응 #1370867

반응 방정식

dithietane

methylene bromide

triethylamine

potassium phenylthiomethyldithiocarbamate

→

2-(Phenylthiomethylimino)-1,3-dithietane

용매

dimethylformamide

water

반응 조건

후처리

1. 1
   workup.ADDITIONTo a mixture of 28.2 g
2. 2
   추출extracted with ethylene chloride
3. 3
   세척The ethylene chloride mixture was washed with water
4. 4
   기타dried
5. 5
   여과The resulting salt was collected by filtration
6. 6
   세척washed with acetone
7. 7
   workup.DISSOLUTIONof chloroform, dissolved
8. 8
   기타removal and concentration of the chloroform layer
9. 9
   기타gave 8.5 g

실험 절차

To a mixture of 28.2 g. of methylene bromide and 10.9 g. of triethylamine in 250 ml. of dimethylformamide was added, in portions, 27.3 g. of potassium phenylthiomethyldithiocarbamate keeping the reaction temperature below 30°C. by cooling. After another 2 hours, the mixture was poured into water and extracted with ethylene chloride. The ethylene chloride mixture was washed with water, dried, and saturated with dry hydrogen chloride. The resulting salt was collected by filtration and washed with acetone. The salt, on stirring with a mixture of 100 ml. of water and 300 ml. of chloroform, dissolved and removal and concentration of the chloroform layer gave 8.5 g. of the dithietane as a white solid, m.p. 50°-52°C.

출처