反应详情

Add Lawesson's Reagent (12.25 g, 30.29 mmol) to a solution of benzyl N-[(3R)-2-oxo-1,3,4,5-tetrahydro-1-benzazepin-3-yl]carbamate (9.4 g, 30.29 mmol) in tetrahydrofuran (470 mL) and stir the reaction under nitrogen for approximately 16 hours at ambient temperature. Remove the precipitate by filtration and discard it. Concentrate the filtrate under reduced pressure and dissolve the residue in ethyl acetate. Wash with water and brine, dry over sodium sulfate, and concentrate the organic layer under reduced pressure to give a thick, yellow oil. Add ether to the thick oil and scratch it to form a solid. Collect the solid by filtration and wash it with ether. Triturate the solid with ether and collect it by filtration to give the title compound (7.28 g, 74%) as a white solid: MS (m/z): 349 (M+23).

1. customthe reaction under nitrogen for approximately 16 hours at ambient temperature
2. customRemove the precipitate
3. filtrationby filtration
4. concentrationConcentrate the filtrate under reduced pressure
5. dissolutiondissolve the residue in ethyl acetate
6. washWash with water and brine
7. dry with materialdry over sodium sulfate
8. concentrationconcentrate the organic layer under reduced pressure
9. customto give a thick, yellow oil
10. customCollect the solid
11. filtrationby filtration
12. washwash it with ether
13. customTriturate the solid with ether
14. customcollect it
15. filtrationby filtration