Hydrochloric Acid → HCID 21471671、化合物
反応式
C(OC([NH:8][C:9]1[N:14]=[CH:13][C:12]([C:15]([N:17]2[CH2:22][CH2:21][CH:20]([N:23]3[CH2:28][CH2:27][CH:26]([N:29]4[C:33]5[CH:34]=[CH:35][CH:36]=[CH:37][C:32]=5[NH:31][C:30]4=[O:38])[CH2:25][CH2:24]3)[CH2:19][CH2:18]2)=[O:16])=[CH:11][N:10]=1)=O)(C)(C)C.[ClH:39]>C(OCC)(=O)C>[ClH:39].[ClH:39].[NH2:8][C:9]1[N:10]=[CH:11][C:12]([C:15]([N:17]2[CH2:18][CH2:19][CH:20]([N:23]3[CH2:28][CH2:27][CH:26]([N:29]4[C:33]5[CH:34]=[CH:35][CH:36]=[CH:37][C:32]=5[NH:31][C:30]4=[O:38])[CH2:25][CH2:24]3)[CH2:21][CH2:22]2)=[O:16])=[CH:13][N:14]=1参加物
4
反応条件
- 温度
- -50 °C
実験手順
The 1,3-dihydro-1-{1-[1-(2-tert-butoxycarbonylamino-5-pyrimidinylcarbonyl)piperidin-4-yl]piperidin-4-yl}-2H-benzimidazol-2-one was dissolved in ethyl acetate, cooled to -50° C. and treated with a stream of HCl gas for 2 min. The reaction mixture was allowed to warm to room temperature and stir for several hours, and then concentrated to dryness under reduced pressure. The product 1,3-dihydro-1-{1-[1-(2-amino-5-pyrimidinecarbonyl)piperidin-4-yl]piperidin-4-yl}-2H-benzimidazol-2-one dihydrochloride salt, was obtained as white solid: Analysis calculated for C22H25N7O2.2 HCl.1.0 C7H8.3.0 H2O: C: 54.38, H: 6.77, N: 15.31; found C: 54.31, H: 6.48, N: 15.23.