Beta-Nitrostyrene → alpha-(Nitromethyl)benzyl dimethyldithiocarbamate

참여 물질

반응 단계

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° C. (prior sintering). The infrared spectrum was essentially identical to the spectrum of analytically pure material.

출처 및 근거