反应详情

To a stirred solution of morpholine (201 mL, 2295 mmol) in water (2 L) was added carbon disulfide (0.138 L, 2295.67 mmol) under nitrogen. Sodium hydroxide (96 g, 2410 mmol in solution in 1 L of water) was then added dropwise. The resulting mixture was stirred at room temperature for 1 h, then cooled to 5° C. with an ice bath and dimethyl sulphate (217 mL, 2295 mmol) was added dropwise. The mixture was stirred 1 h at room temperature, the obtained solid was collected by filtration, washed with water (2×1 L) and dried under vacuum over phosphorus pentoxide at 50° C. to give methyl morpholine-4-carbodithioate (360 g, 88%). Proton NMR Spectrum: (CDCl3): 2.68 (s, 3H), 3.71-3.84 (m, 4H), 4.02 (bs, 2H), 4.30 (bs, 2H).

1. temperaturecooled to 5° C. with an ice bath
2. stirringThe mixture was stirred 1 h at room temperature
3. filtrationthe obtained solid was collected by filtration
4. washwashed with water (2×1 L)
5. dry with materialdried under vacuum over phosphorus pentoxide at 50° C.