反应详情

A solution of (E)-N-methyl-N-(3-methylbenzofuran-2-ylmethyl)-3-(2,3,4,5-tetrahydro-1H-pyrido[2,3-e][1,4]diazepin-7-yl)acrylamide (0.21 g, 0.56 mmol) in CH2Cl2 (5 mL) was treated with anhydrous HCl (0.56 mL of a 1.0 M solution in Et2O, 0.56 mmol). After stirring for 5 min, the mixture was diluted with Et2O (50 mL), allowed to stir for 30 min and sonicated for 5 min. The solid was isolated by filtration, washed with Et2O, and dried under vacuum at 50° C. for 4 days to give the title compound (0.22 g, 97%) as an off-white powder and as a mixture of amide rotamers: 1H NMR (300 MHz, DMSO-d6) δ 9.66 (br s, 2H), 8.36-8.33 (m, 1H), 8.14 (s, 1H), 7.58-7.07 (m, 7H), 4.98-4.79 (m, 2H), 4.26 (s, 2H), 3.51 (s, 2H), 3.33 (s, 2H), 3.17-2.91 (m, 3H), 2.27 (s, 3H); MS (ESI) m/e 377 (M+H)+.

1. stirringto stir for 30 min
2. customsonicated for 5 min
3. customThe solid was isolated by filtration
4. washwashed with Et2O
5. customdried under vacuum at 50° C. for 4 days