反应详情

Potassium diphenylmethyldithiocarbamate was prepared from diphenylmethyl isothiocyanate and potassium hydrosulfide in a t-butyl alcohol acetone mixture. A mixture of 29.7 g. of this salt, 26.1 g. of methylene bromide, and 10.1 g. of triethylamine in 200 ml. of dimethylformamide was stirred for about 1 hour keeping the initial reaction temperature below 30°C. by cooling. The mixture was poured into ice-water, partitioned into ethylene chloride, and gave 24.0 g. of crude product upon evaporation of the ethylene chloride. Purification by dry column chromatography on silica gel using 20% methylene chloride in hexane for developing gave 5.5 g. of solids which were recrystallized from isopropyl alcohol to give 4.4 g. of white crystals, m.p. 106.5°-107.5°C.

1. additionA mixture of 29.7 g
2. customreaction temperature below 30°C.
3. temperatureby cooling
4. custompartitioned into ethylene chloride
5. customgave 24.0 g
6. customof crude product upon evaporation of the ethylene chloride
7. customPurification
8. dry with materialby dry column chromatography on silica gel using 20% methylene chloride in hexane
9. customfor developing gave 5.5 g
10. customof solids which were recrystallized from isopropyl alcohol
11. customto give 4.4 g