Nicotinic Acid → 2-Benzoyl amino-pentane dioic acid dimethyl ester
反応式
[CH:1]1[CH:6]=N[CH:4]=[C:3]([C:7]([OH:9])=O)[CH:2]=1.[CH3:10]N1CCOCC1.CCN=C=NCCCN(C)C.Cl.[CH3:29][O:30][C:31](=[O:40])[C@H:32]([CH2:34][CH2:35][C:36]([O:38][CH3:39])=[O:37])[NH2:33]>C(Cl)Cl>[CH3:29][O:30][C:31](=[O:40])[C:32]([NH2:33])([C:7](=[O:9])[C:3]1[CH:2]=[CH:1][CH:6]=[CH:10][CH:4]=1)[CH2:34][CH2:35][C:36]([O:38][CH3:39])=[O:37]参加物
6
反応条件
- 温度
- 25 °C
実験手順
To a solution of niacin (1.4 g, 11.42 mmol) in DCM (20 mL) were added N-methyl morpholine (3.76 mL, 34.2 mmol), EDCI.HCl (4.36 g, 34.2 mmol) and L-glutamic acid dimethyl ester (2.0 g, 11.42 mmol). The mixture was allowed to stir at room temperature (25° C.) over 3 h under nitrogen atmosphere. The resulting mixture was diluted with DCM (100 mL), washed with water (3×50 mL) and dried over sodium sulphate. The crude product obtained upon evaporation of the solvent was further purified by silica gel column chromatography to obtain required product as pale yellow oil (3.1 g, 73%).
後処理
- washwashed with water (3×50 mL)
- dry with materialdried over sodium sulphate
- customThe crude product obtained upon evaporation of the solvent
- customwas further purified by silica gel column chromatography
出典と根拠
- ORDレコード
- ord-466ad572ab5643d8b303080aa2f9a680
- 出典データセット
- uspto-grants-2014_09
- 特許番号
- US08846721B2
反応ノート
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