反应详情

While cooling and stirring, 20 g. (0.20 mole) of 2,2-dimethyloxazolidine (preparation described by E. Bergmann et. al., J. Am. Chem. Soc. 75, 358 (1953)) was added to a solution of 15.2 g. (0.20 mole) carbon disulfide in 150 g. pyridine. To the stirring solution was added 18.3 g. (0.10 mole) of anhydrous zinc acetate at 25°-30°C. After standing overnight at room temperature, filtration gave 15.2 g. of the crude product; vacuum-concentration of the filtrate and ethanol-dilution of the residue gave an additional 10.4 g. After combining and vacuum-drying of the crude product at 100°C there was obtained 17.8 g. of the desired carbodithioate melting at 188°- 190°C (decomp.). A small sample, dissolved in hot chloroform and precipitated by hexane (m. 192°- 3°C decomp.) had the following analysis: Found: C, 34.22; H, 4.47; N, 6.84; Zn, 15.20%. Calcd for C12H20N2O2S 4 Zn: C, 34.50; H, 4.79; N, 6.71; Zn, 15.67%.

1. temperatureWhile cooling
2. additionTo the stirring solution was added 18.3 g
3. customat 25°-30°C
4. filtrationfiltration
5. customgave 15.2 g
6. dry with materialvacuum-drying of the crude product at 100°C
7. customthere was obtained 17.8 g
8. customprecipitated by hexane (m. 192°- 3°C decomp.)