Hydrochloric Acid → HCID 136367008、化合物

反応式

[ClH:1].CCOCC.[F:7][C:8]1[CH:13]=[CH:12][CH:11]=[C:10]([OH:14])[C:9]=1[C:15]1[N:24]=[C:23]([N:25]2[CH2:29][CH2:28][C@@H:27]([NH:30][C:31]([CH:33]3[CH2:35][CH2:34]3)=[O:32])[CH2:26]2)[C:22]2[C:17](=[CH:18][C:19]([CH3:36])=[CH:20][CH:21]=2)[N:16]=1>C(Cl)Cl>[ClH:1].[F:7][C:8]1[CH:13]=[CH:12][CH:11]=[C:10]([OH:14])[C:9]=1[C:15]1[N:24]=[C:23]([N:25]2[CH2:29][CH2:28][C@@H:27]([NH:30][C:31]([CH:33]3[CH2:34][CH2:35]3)=[O:32])[CH2:26]2)[C:22]2[C:17](=[CH:18][C:19]([CH3:36])=[CH:20][CH:21]=2)[N:16]=1

参加物

実験手順

A 2 M HCl solution in ether (0.16 mL, 0.32 mmol) was added to a solution of N-((R)-1-(2-(2-fluoro-6-hydroxyphenyl)-7-methylquinazolin-4-yl)pyrrolidin-3-yl)cyclopropanecarboxamide (133 mg, 0.32 mmol) in CH2Cl2 (4 mL) under an N2 atmosphere. Additional ether was then added (15 mL) and the reaction mixture was stirred for an hour. The formed precipitate was then filtered and dried to afford N-((R)-1-(2-(2-fluoro-6-hydroxyphenyl)-7-methylquinazolin-4-yl)pyrrolidin-3-yl)cyclopropanecarboxamide hydrochloride (135 mg, 95%). LC/MS: m/z 407.5 (M+H)+ at 2.07 min (10%-99% CH3CN (0.035% TFA)/H2O (0.05% TFA)). 1H NMR (400 MHz, DMSO-d6) δ 8.32 (d, J=7.6 Hz, 1H), 7.56-7.58 (m, 2H), 7.43-7.49 (m, 1H), 6.83-6.88 (m, 2H), 3.94-4.41 (m, 5H), 2.52 (s, 3H), 2.25-2.36 (m, 1H), 1.91-2.13 (m, 1H), 1.47-1.54 (m, 1H), 0.63-0.69 (m, 4H)