Potassium Carbonate → Tert-butyl 2-((3-(4-benzylpiperidin-1-yl)propyl)(2-tert-butoxybenzyl)amino)ethylcarbamate
反応式
[C:1]([O:5]C1C=CC=CC=1CN(CC1C=CC=CN=1)CCCN1CCC(C2C=CC=CC=2)CC1)([CH3:4])([CH3:3])[CH3:2].[CH2:36]([CH:43]1[CH2:48][CH2:47][NH:46][CH2:45][CH2:44]1)[C:37]1[CH:42]=[CH:41][CH:40]=[CH:39][CH:38]=1.[C:49]([O:53][C:54]1[CH:74]=[CH:73][CH:72]=[CH:71][C:55]=1[CH2:56][N:57]([CH2:67][CH2:68][CH2:69]Cl)[CH2:58][CH2:59][NH:60][C:61](=[O:66])C(C)(C)C)([CH3:52])([CH3:51])[CH3:50].C([O-])([O-])=O.[K+].[K+]>>[CH2:36]([CH:43]1[CH2:48][CH2:47][N:46]([CH2:69][CH2:68][CH2:67][N:57]([CH2:56][C:55]2[CH:71]=[CH:72][CH:73]=[CH:74][C:54]=2[O:53][C:49]([CH3:50])([CH3:51])[CH3:52])[CH2:58][CH2:59][NH:60][C:61](=[O:66])[O:5][C:1]([CH3:4])([CH3:3])[CH3:2])[CH2:45][CH2:44]1)[C:37]1[CH:42]=[CH:41][CH:40]=[CH:39][CH:38]=1参加物
反応物 4
生成物 1
実験手順
The same procedure as described for compound 20 was applied to 4-benzylpiperidine (0.46 g, 2.63 mmol), compound 23 (0.7 g, 1.75 mmol), KI (0.87 g, 5.25 mmol) and K2CO3 (1.21 g, 8.75 mmol). The residue was purified on a silica gel TLC plate that was developed in 5% methanolic NH3 (7 M NH3 in methanol/95% CH2Cl2. The product was isolated as yellow oil (80% yield). 1H NMR (CDCl3) δ 7.373 (d, 1H, Ar), 7.264 (m, 2H, Ar), 7.176 (t, 1H, Ar), 7.137 (d, 2H, Ar), 7.137 (d, 2H, Ar), 7.108 (d, 1H, Ar), 7.021 (dd, 1H, Ar), 6.985 (t, 1H, Ar), 3.577 (s, 2H, —CH2—), 3.167 (d, 2H, —CH2—), 2.892 (d, 2H, —CH2—), 2.524 (d, 2H, —CH2—), 2.498 (t, 2H, —CH2—), 2.453 (t, 2H, —CH2—), 2.290 (t, 2H, —CH2—), 1.839 (t, 2H, —CH2—), 1.657 (m, 2H, —CH2—), 1.618 (d, 2H, —CH2—), 1.517 (m, 1H, —CH—), 1.426 (s, 9H, —C(CH3)3, 1.376 (s, 9H, —C(CH3)3, 1.329 (overlapped m, 4H). Mass Spec.=538.77 (M+H)+.
後処理
- customThe residue was purified on a silica gel TLC plate that
出典と根拠
- ORDレコード
- ord-e6466a842207460b93b3a12d7894ee7c
- 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…