反应详情

A mixture of N-butyl glycine (12.0 g), 5-chloro-2-methylphenyl-isothiocyanate (9.15 g), triethyl amine (12.0 g) and chloroform (200 mL) was heated at reflux for 5 hours. The solvent was evaporated. The residue was treated with diethyl ether (400 mL). The mixture was filtered. The solid was washed with diethyl ether then discarded. The filtrate was evaporated to dryness. Crystallization from ethanol afforded the title compound (6.0 g) as a tan solid, m.p. 102°-103° C. Anal. Calcd. for. C14H17Cl N2 O S: C, 56.65; H, 5.77; N, 9.44. Found: C, 56.41; H, 5.97; N, 9.36. Mass spectrum (EI, M.+) m/z 296/298.

1. temperaturewas heated
2. temperatureat reflux for 5 hours
3. customThe solvent was evaporated
4. additionThe residue was treated with diethyl ether (400 mL)
5. filtrationThe mixture was filtered
6. washThe solid was washed with diethyl ether
7. customThe filtrate was evaporated to dryness
8. customCrystallization from ethanol