Hydrochloric Acid → 3-Amino-N-{[5-chloro-2-(methoxypropyl)-1-oxidopyridin-4-yl]methyl}-N-cyclopropyl-2-{4-[2-(2,6-dichloro-4-methylphenoxy)ethoxy]benzyl}propanamide
反応式
[Cl:1][C:2]1[C:3]([CH2:14][N:15]([CH:48]2[CH2:50][CH2:49]2)[C:16](=[O:47])[CH:17]([CH2:27][C:28]2[CH:33]=[CH:32][C:31]([O:34][CH2:35][CH2:36][O:37][C:38]3[C:43]([Cl:44])=[CH:42][C:41]([CH3:45])=[CH:40][C:39]=3[Cl:46])=[CH:30][CH:29]=2)[CH2:18][NH:19]C(=O)OC(C)(C)C)=[CH:4][C:5]([CH2:9][CH2:10][CH2:11][O:12][CH3:13])=[N+:6]([O-:8])[CH:7]=1.Cl>C(Cl)Cl>[NH2:19][CH2:18][CH:17]([CH2:27][C:28]1[CH:33]=[CH:32][C:31]([O:34][CH2:35][CH2:36][O:37][C:38]2[C:43]([Cl:44])=[CH:42][C:41]([CH3:45])=[CH:40][C:39]=2[Cl:46])=[CH:30][CH:29]=1)[C:16]([N:15]([CH2:14][C:3]1[C:2]([Cl:1])=[CH:7][N+:6]([O-:8])=[C:5]([CH2:9][CH2:10][CH2:11][O:12][CH3:13])[CH:4]=1)[CH:48]1[CH2:50][CH2:49]1)=[O:47]参加物
4
実験手順
To a CH2Cl2 solution (0.07 M) of tert-butyl (3-[{[5-chloro-2-(methoxypropyl)-1-oxidopyridin-4-yl]methyl}(cyclopropyl)amino]-2-{4-[2-(2,6-dichloro-4-methylphenoxy)ethoxy]benzyl}-3-oxopropyl)carbamate from the previous step (1 eq.) was added HCl (4.0 M dioxane solution, 30 eq.). The resulting solution was stirred at RT for 16 h. Following the removal of the volatiles in vacuo, the resulting residue was directly subjected to column chromatography (SiO2, 95:5 (v/v) CH2Cl2: 2.0 M NH3 in MeOH) to afford the title compound as an oil. MS (ESI+): 651.
後処理
- customthe removal of the volatiles in vacuo
出典と根拠
- ORDレコード
- ord-4261ab71dd824d9599905af6b70d1698
- 出典データセット
- uspto-grants-2011_11
- 特許番号
- US08063105B2
反応ノート
読み込み中…