反应详情

A solution of (E)-3-[4-(3-Morpholin-4-yl-propyl)-2-oxo-2,3,4,5-tetrahydro-1H-pyrido[2,3-e][1,4]diazepin-7-yl]acrylic acid tert-butyl ester (2.21 g, 5.30 mmol) in CH2Cl2 (20 mL) was treated with TFA (20 mL). After stirring at room temperature for 30 min, the solution was concentrated in vacuo. The resulting oil was treated with anhydrous HCl (50 mL of a 4.0 M solution in dioxane, 200 mmol) and the mixture was sonicated for 1.5 h. The mixture was diluted with Et2O (200 mL) and sonicated for 15 min. The solid was isolated by filtration, washed with Et2O, and dried under vacuum at 50° C. for 5 h to give the title compound (3.08 g, quantitative) as an off-white solid: 1H NMR (500 MHz, DMSO-d6) δ 11.23 (br s, 2H), 8.74 (s, 1H), 8.36 (s, 1H), 7.63 (d, J=15.9, 1H), 6.63 (d, J=16.0 Hz, 1H), 4.33 (br s, 2H), 3.90 (br s, 6H), 3.24 (m, 8H), 2.22 (br s, 2H); MS (ESI) m/e 361 (M+H)+.

1. concentrationthe solution was concentrated in vacuo
2. additionThe resulting oil was treated with anhydrous HCl (50 mL of a 4.0 M solution in dioxane, 200 mmol) and the mixture
3. customwas sonicated for 1.5 h
4. additionThe mixture was diluted with Et2O (200 mL)
5. customsonicated for 15 min
6. customThe solid was isolated by filtration
7. washwashed with Et2O
8. customdried under vacuum at 50° C. for 5 h