反应详情

A mixture of the crude N-ethyl glycine (18.4 g), 2,6-diisopropylphenyl-isothiocyanate (21.9 g), triethyl amine (20.2 g) and chloroform (300 mL) was heated at reflux for 18 hours. The solvent was evaporated. The residue was dissolved in ethyl acetate (400 mL) and water (300 mL). The organic phase was washed with 1N HCl (2×300 mL), then evaporated to dryness. Purification was achieved through crystallization from ethanol. The title compound (8.2 g) was obtained as a light yellow solid, m.p. 159°-161° C. Anal. Calcd. for. C17H24N2OS: C, 67.07; H, 7.94; N, 9.20. Found: C, 66.92; H, 8.03; N, 9.13. Mass spectrum (PBEI, M.+) m/z 304.

1. temperaturewas heated
2. temperatureat reflux for 18 hours
3. customThe solvent was evaporated
4. dissolutionThe residue was dissolved in ethyl acetate (400 mL)
5. washThe organic phase was washed with 1N HCl (2×300 mL)
6. customevaporated to dryness
7. customPurification
8. customwas achieved through crystallization from ethanol