反应详情

To 5-(4-phenoxyphenyl)-7-(4-piperidyl)-7H-pyrrolo[2,3-d]pyrimidin-4-ylamine (433258) (200 mg) in EtOAc/MeOH (15 ml, 1:1) was added ether.HCl solution (1.0 M, 3 ml). The resulting white precipitate was filtered under a stream of nitrogen and dried in vacuo for 6 hr to leave 5-(4-phenoxyphenyl)-7-(4-piperidyl)-7H-pyrrolo[2,3-d]pyrimidin-4-ylamine dihydrochloride (1.4 hydrate) as a white solid (120 mg), m.pt. 304° C (dec.). 1H NMR (D2O, 250 MHz) 8.48(1H, s), 7.69 (1H, s), 7.50-7.58 (4H, m), 7.18-7.34 (5H, m), 5.16 (1H, m), 3.81 (2H, d), 3.46 (2H, m), 2.49 (4H, m).). IR (KBr disc): 3937, 1657, 1231 cm−1.

1. filtrationThe resulting white precipitate was filtered under a stream of nitrogen
2. customdried in vacuo for 6 hr