反応式
[OH:1][C:2]1[CH:3]=[CH:4][C:5]([C:8]([OH:10])=O)=[N:6][CH:7]=1.C(N(C(C)C)CC)(C)C.O.ON1C2C=CC=CC=2N=N1.CCN=C=NCCCN(C)C.Cl.[C:43]1([CH2:49][CH2:50][CH2:51][NH2:52])[CH:48]=[CH:47][CH:46]=[CH:45][CH:44]=1>ClCCl>[C:43]1([CH2:49][CH2:50][CH2:51][NH:52][C:8]([C:5]2[CH:4]=[CH:3][C:2]([OH:1])=[CH:7][N:6]=2)=[O:10])[CH:48]=[CH:47][CH:46]=[CH:45][CH:44]=1参加物
7
反応物 5
生成物 1
試薬・触媒・溶媒 1
実験手順
To a solution of 5-hydroxypyridine-2-carboxylic acid (0.103 g, 0.74 mmol) in dichloromethane was added diisopropylethylamine (0.279 mL, 1.6 mmol), followed by 1-hydroxybenzotriazole monohydrate (0.012 g, 0.8 mmol) and EDCl (0.153 g, 0.8 mmol). The resulting mixture was stirred for 15 minutes and 3-phenyl-1-propylamine (0.108 g, 0.8 mmol) was added. After stirring for 22 h, the reaction mixture was diluted with dichloromethane (80 mL), washed with water, dried over anhydrous Na2SO4 and concentrated in vacuo. Purification by column chromatography afforded 5-hydroxypyridine-2-carboxylic acid (3-phenylpropyl)amide as white crystals (0.116 g, 61% yield). MS (ES+) m/z 257.2 (M+1).
後処理
- stirringAfter stirring for 22 h
- washwashed with water
- dry with materialdried over anhydrous Na2SO4
- concentrationconcentrated in vacuo
- customPurification by column chromatography
出典と根拠
- ORDレコード
- ord-a9fa6b3d185c4673b13359a4b947e175
- 出典データセット
- uspto-grants-2013_02
- 特許番号
- US08383628B2
関連ノート
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