Potassium Carbonate → Tert-butyl-2-((6-(4-benzylpiperidin-1-yl)hexyl)(2-tert-butoxybenzyl)amino)ethylcarbamate
反応式
[C:1]([O:5][C:6]1[CH:41]=[CH:40][CH:39]=[CH:38][C:7]=1[CH2:8][N:9]([CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][N:26]1[CH2:31][CH2:30][CH:29](C2C=CC=CC=2)[CH2:28][CH2:27]1)[CH2:10][CH2:11][NH:12][C:13](=[O:19])[O:14][C:15]([CH3:18])([CH3:17])[CH3:16])([CH3:4])([CH3:3])[CH3:2].BrCCCCCCN([CH2:60][C:61]1[CH:66]=[CH:65][CH:64]=[CH:63][C:62]=1OC(C)(C)C)CCNC(=O)OC(C)(C)C.C(C1CCNCC1)C1C=CC=CC=1.C([O-])([O-])=O.[K+].[K+]>>[C:15]([O:14][C:13](=[O:19])[NH:12][CH2:11][CH2:10][N:9]([CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][N:26]1[CH2:27][CH2:28][CH:29]([CH2:60][C:61]2[CH:66]=[CH:65][CH:64]=[CH:63][CH:62]=2)[CH2:30][CH2:31]1)[CH2:8][C:7]1[CH:38]=[CH:39][CH:40]=[CH:41][C:6]=1[O:5][C:1]([CH3:3])([CH3:2])[CH3:4])([CH3:17])([CH3:16])[CH3:18]参加物
反応物 4
生成物 1
実験手順
The same procedure as described for compound 16 was applied to starting material 15 (2.4 g, 5.89 mmol), 4-benzylpiperidine (2.06 g, 11.78 mmol) and K2CO3 (0.814 g, 5.89 mmol). Purification was carried out on a silica gel TLC plate that was developed in with a 3% methanolic NH3 (7 M NH3 in methanol/97% CH2Cl2. The product was isolated as pale yellow oil (58%). 1H NMR (CDCl3) δ 7.328 (dd, 1H, Ar), 7.211 (t, 2H, Ar), 7.132 (t, 1H, Ar), 7.077 (m, 3H, Ar), 6.951 (m, 2H, Ar), 3.576 (s, 2H, —CH2—), 3.302 (d, 2H, —CH2—), 3.112 (m, 2H, —CH2—), 2.729 (m, 2H, —CH2—), 2.525 (m, 6H), 2.395 (m, 2H, —CH2—), 1.819 (m, 2H, —CH2—), 1.724 (m, 5H), 1.424 (m, 2H, —CH2—), 1.356 (s, 9H, —C(CH3)3), 1.325 (s, 9H, —C(CH3)3), 1.224 (s(br), 4H, —CH2—CH2—). Mass Spec.=579.86 (M+H)+.
後処理
- customPurification
出典と根拠
- ORDレコード
- ord-314aaa1386a8496e997afe0b1002ae86
- 出典データセット
- uspto-grants-2014_06
- 特許番号
- US08747810B2
反応ノート
読み込み中…