反応式
[OH:1][C@H:2]([C:19]1[CH:24]=[CH:23][C:22]([OH:25])=[C:21]([CH2:26][OH:27])[CH:20]=1)[CH2:3][NH:4][C@H:5]([CH3:18])[CH2:6][C:7]1[CH:8]=[C:9]([CH2:13][CH2:14][C:15](O)=[O:16])[CH:10]=[CH:11][CH:12]=1.[F:28][C:29]1[CH:36]=[CH:35][CH:34]=[C:33]([Cl:37])[C:30]=1[CH2:31][NH2:32].C(N(CC)CC)C>CN(C)C=O>[NH3:4].[Cl:37][C:33]1[CH:34]=[CH:35][CH:36]=[C:29]([F:28])[C:30]=1[CH2:31][NH:32][C:15](=[O:16])[CH2:14][CH2:13][C:9]1[CH:10]=[CH:11][CH:12]=[C:7]([CH2:6][C@H:5]([NH:4][CH2:3][C@H:2]([OH:1])[C:19]2[CH:24]=[CH:23][C:22]([OH:25])=[C:21]([CH2:26][OH:27])[CH:20]=2)[CH3:18])[CH:8]=1参加物
6
反応物 3
生成物 2
試薬・触媒・溶媒 1
実験手順
A solution of 3-{3-[(2R)-2-({(2R)-2-hydroxy-2-[4-hydroxy-3-(hydroxymethyl)phenyl]ethyl}amino)propyl]phenyl}propanoic acid (Preparation 60) (150 mg, 0.29 mmol), O-(1H-benzotrizol-1-yl)-N,N,N′,N′-tetramethyluronium hexafluorophosphate (133 mg, 0.35 mmol), 2-fluoro-6-chlorobenzylamine (56 mg, 0.35 mmol) and triethylamine (0.12 ml, 0.88 mmol) were stirred at room temperature for 16 hours in N,N-dimethylformamide (3 ml). The solvent was removed in vacuo and the resulting brown oil was purified by flash column chromatography on silica gel eluting with dichloromethane:methanol:880 ammonia (98:2:0.2 followed by 94:6:0.6 by volume) to give the title compound as a white foam (30 mg).
後処理
- customThe solvent was removed in vacuo
- customthe resulting brown oil was purified by flash column chromatography on silica gel eluting with dichloromethane
出典と根拠
- ORDレコード
- ord-5e9630c9cf1e43349515ed3c6211291d
- 出典データセット
- uspto-grants-2007_09
- 特許番号
- US07268147B2
関連ノート
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