反应详情

Combine benzyl N-[(3R)-2-thioxo-1,3,4,5-tetrahydro-1-benzazepin-3-yl]carbamate (8.71 g, 26.68 mmol), mercury dichloride (HgCl2) (9.42 g, 34.69 mmol), and aminoacetaldehyde dimethyl acetal (11.65 mL, 106.73 mmol;) in tetrahydrofuran (250 mL) and heat to 55° C. for 20 minutes. Cool the mixture to ambient temperature and filter it through diatomaceous earth. Wash the cake with THF and ethyl acetate and concentrate the filtrate under reduced pressure. Dissolve the resulting oil in dichloromethane, wash with warm water (4×) and brine, dry over sodium sulfate, and concentrate the organic layer under reduced pressure to give the title compound (9.78 g, 92%) as a solid: MS (m/z): 398 (M+1).

1. filtrationfilter it through diatomaceous earth
2. washWash the cake with THF and ethyl acetate
3. concentrationconcentrate the filtrate under reduced pressure
4. dissolutionDissolve the resulting oil in dichloromethane
5. washwash with warm water (4×) and brine
6. dry with materialdry over sodium sulfate
7. concentrationconcentrate the organic layer under reduced pressure