反応式
[H-].[Na+].[N:3]1([CH:8]([C:10]2[CH:11]=[C:12]([CH:18]=[CH:19][CH:20]=2)[O:13][CH2:14][CH2:15][CH2:16][NH2:17])[CH3:9])[CH2:7][CH2:6][CH2:5][CH2:4]1.[OH:21][C:22]([CH3:28])([CH3:27])[C:23](OC)=[O:24]>CS(C)=O>[OH:21][C:22]([CH3:28])([CH3:27])[C:23]([NH:17][CH2:16][CH2:15][CH2:14][O:13][C:12]1[CH:18]=[CH:19][CH:20]=[C:10]([CH:8]([N:3]2[CH2:4][CH2:5][CH2:6][CH2:7]2)[CH3:9])[CH:11]=1)=[O:24]参加物
実験手順
43 mg of 50% sodium hydride was suspended in 0.5 ml of dry dimethylsulfoxide, and with stirring under ice cooling, a solution of 200 mg of 3-[3-[1-(1-pyrrolidinyl)ethyl]phenoxy]propylamine in 0.5 ml of dimethylsulfoxide was added dropwise. The mixture was stirred at room temperature for 20 minutes. Then, 105 mg of methyl α-hydroxyisobutyrate was added dropwise, and the mixture was stirred at room temperature for 1 hour. Ice water was added to the reaction mixture, and the mixture was extracted with chloroform. The organic layer was washed with water, and dried over anhydrous sodium sulfate. The solvent was distilled off, and the resulting crude oil was separated and purified by TLC (developing solvent: chloroform/methanol=9/l) to afford 71 mg of N-(2-hydroxy-2-methylpropionyl)-3-[3-[1-(1-pyrrolidinyl)ethyl]phenoxy]propylamine as an oil.
後処理
- stirringThe mixture was stirred at room temperature for 20 minutes
- stirringthe mixture was stirred at room temperature for 1 hour
- extractionthe mixture was extracted with chloroform
- washThe organic layer was washed with water
- dry with materialdried over anhydrous sodium sulfate
- distillationThe solvent was distilled off
- customthe resulting crude oil was separated
- custompurified by TLC (developing solvent: chloroform/methanol=9/l)
出典と根拠
- ORDレコード
- ord-575e106b89bf4857a0fee465a3630121
- 出典データセット
- uspto-grants-1981_10
- 特許番号
- US04293557
関連ノート
読み込み中…