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 one 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