反应详情

A mixture of the crude N-isopropyl glycine (21.2 g), 5-chloro-2-methylphenyl-isothiocyanate (18.3 g), triethyl amine (21.0 g) and chloroform (300 mL) was heated at reflux for 4 hours. The solvent was evaporated. The residue was dissolved in ethyl acetate (400 mL) and water (300 mL). The organic phase was washed with 2N HCl (2×300 mL), then with water. The organic phase was dried over anhydrous magnesium sulfate and evaporated to dryness. Crystallization from ethanol afforded the title compound (15.4 g) as a peach solid, m.p. 142°-144° C. Anal. Calcd. for. C13H15Cl N2O S: C, 55.21; H, 5.35; N, 9.91. Found: C, 55.07; H, 5.20; N, 9.82. Mass spectrum (+FAB, [M+H]+) m/z 283/285.

1. temperaturewas heated
2. temperatureat reflux for 4 hours
3. customThe solvent was evaporated
4. dissolutionThe residue was dissolved in ethyl acetate (400 mL)
5. washThe organic phase was washed with 2N HCl (2×300 mL)
6. dry with materialThe organic phase was dried over anhydrous magnesium sulfate
7. customevaporated to dryness
8. customCrystallization from ethanol