反应详情

Dimethylammonium dimethyldithiocarbamate (16.6 grams, 0.10 mole), carbon disulfide (7.6 grams, 0.10 mole), and β-nitrostyrene (14.9 grams, 0.10 mole) were dissolved in methanol (50 ml.). A rapid exothermic reaction ensued and the product precipitated. The reaction temperature was held to 35° C. with ice cooling. After several hours at 25° C., the product was filtered off, washed with methanol, and dried in air. The crude product melted at ca. 103° C.-110° C. and weighed 22.9 grams (85%). Recrystallizations from hot methanol and from acetone-2-propanol solution (without heating) gave 13.8 grams of α-(nitromethyl)-benzyl dimethyldithiocarbamate melting at 104° C.-108.5° C. (prior sintering). The infrared spectrum was essentially identical to the spectrum of analytically pure material.

1. customA rapid exothermic reaction
2. customthe product precipitated
3. customwas held to 35° C. with ice cooling
4. waitAfter several hours at 25° C.
5. filtrationthe product was filtered off
6. washwashed with methanol
7. customdried in air
8. customRecrystallizations from hot methanol