反应详情

A solution of (7-bromo-2-oxo-1,2,3,5-tetrahydro-pyrido[2,3-e][1,4]diazepin-4-yl)acetic acid tert-butyl ester (1.61 g, 4.52 mmol) in CH2Cl2 (20 mL) was treated with TFA (15 mL). After stirring at room temperature for 1 h, the solution was concentrated in vacuo. The resulting slurry was treated with anhydrous HCl (40 mL of a 4.0 M) and sonicated for 1.5 h, diluted with Et2O and stirred for 1 h. The solid was isolated by filtration, washed with Et2O, and dried under vacuum at 50° C. overnight to give the title compound (1.66 g, 98%) as a white solid: MS (ESI) m/e 300 (M+H)+.

1. concentrationthe solution was concentrated in vacuo
2. additionThe resulting slurry was treated with anhydrous HCl (40 mL of a 4.0 M) and
3. customsonicated for 1.5 h
4. additiondiluted with Et2O
5. stirringstirred for 1 h
6. customThe solid was isolated by filtration
7. washwashed with Et2O
8. customdried under vacuum at 50° C. overnight