反応式
[NH2:1][CH:2]([CH2:6][CH3:7])[C:3]([OH:5])=[O:4].C(N(CC)CC)C.Cl[Si](C)(C)C.[CH:20]1([C:25](Cl)=[O:26])[CH2:24][CH2:23][CH2:22][CH2:21]1>ClCCl.O>[CH:20]1([C:25]([NH:1][CH:2]([CH2:6][CH3:7])[C:3]([OH:5])=[O:4])=[O:26])[CH2:24][CH2:23][CH2:22][CH2:21]1参加物
7
反応条件
- 温度
- 0 °C
実験手順
35 g (339 mmol) 2-aminobutanoic acid and 75.6 g (747 mmol) triethylamine are suspended in 300 ml of dichloromethane and stirred at 0° C. 81 g (747 mmol) chlorotrimethylsilane are added dropwise, then the mixture is stirred for 1 hour at room temperature and 1 hour at 40° C. After cooling down at −10° C., 45 g (339 mmol) cyclopentanecarbonyl chloride are added slowly. The reaction mixture is stirred for 2 hours at −10° C. and then 1 hour at room temperature. At 0° C., 50 ml of water are added. The mixture is diluted with water and dichloromethane, filtered and the solid product washed with water/dichloromethane 9/1, toluene and diethylether.
後処理
- stirringthe mixture is stirred for 1 hour at room temperature and 1 hour at 40° C
- temperatureAfter cooling down at −10° C.
- stirringThe reaction mixture is stirred for 2 hours at −10° C.
- custom1 hour
- customat room temperature
- filtrationfiltered
- washthe solid product washed with water/dichloromethane 9/1, toluene and diethylether
出典と根拠
- ORDレコード
- ord-a0112f11c23a4f8d9cf20e8c9624a0a5
- 出典データセット
- uspto-grants-2006_08
- 特許番号
- US07087605B2
関連ノート
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