反应详情

Step 5: 1 {2-[(4-Chlorobenzyl)-(1-quinazolin-4-yl-piperidine-4-carbonyl)-amino]-ethyl}-carbamic acid tert-butyl ester (190 mg, 0.36 mmol) was dissolved in DCM (5 mL) followed by the addition of 2.0 M HCl in Et2O (2 mL). After being stirred for 12 hours, the mixture was diluted with DCE and concentrated in vacuo. The resulting white solid was then suspended in MeCN and concentrated in vacuo (repeated twice) to give 1-quinazolin-4-yl-piperidine-4-carboxylic acid (2-amino-ethyl)-(4-chlorobenzyl)-amide dihydrochloride as a white powder (120 mg). 1H NMR (DMSO-d6, 400 MHz) δ 8.83 (m, 1H), 8.51 (bs, 2H), 8.20 (m, 2H), 8.01 (m, 2H), 7.71 (m, 1H), 7.48 (d, J=8.3 Hz, 1H), 7.39 (d, J=8.3 Hz, 1H), 7.31 (d, J=8.3 Hz, 1H), 7.25 (d, J=8.3 Hz, 1H), 4.79 (m, 2H), 4.55 (s, 1H), 3.59 (m, 7H), 3.03 (m, 1H), 2.90 (m, 1H), 1.92 (m, 4H). LCMS (APCI+) m/z 424, 426 [M+H]+.

1. concentrationconcentrated in vacuo
2. concentrationconcentrated in vacuo (