反応式
Cl.[NH2:2][CH2:3][C:4]([OH:6])=[O:5].[CH2:7](N(CC)CC)C.[C:14](Cl)(=[O:18])[CH2:15][CH2:16][CH3:17]>C(Cl)Cl>[CH3:7][O:5][C:4](=[O:6])[CH2:3][NH:2][C:14](=[O:18])[CH2:15][CH2:16][CH3:17]参加物
5
実験手順
A suspension of glycine hydrochloride (1.00 g, 7.964 mmol) in methylene chloride (40 mL), cooled to 0° under a nitrogen atmosphere, was treated with triethylamine (4.44 mL, 31.86 mmol) and butyryl chloride (0.93 mL, 8.76 mmol), and the mixture stirred at room temperature for 2.5 hours. The reaction was washed with saturated aqueous sodium bicarbonate (50 mL), water (50 mL) and brine. The organic phase was dried over anhydrous sodium sulfate, filtered and concentrated under vacuum giving the title compound. Purification by silica gel flash chromatography with 25% ethyl acetate/methylene chloride afforded the title compound as a colorless oil (0.776 g, 4.88 mmol, 61%).
後処理
- temperaturecooled to 0° under a nitrogen atmosphere
- washThe reaction was washed with saturated aqueous sodium bicarbonate (50 mL), water (50 mL) and brine
- dry with materialThe organic phase was dried over anhydrous sodium sulfate
- filtrationfiltered
- concentrationconcentrated under vacuum
出典と根拠
- ORDレコード
- ord-529758c4958749dd820eecee4341064e
- 出典データセット
- uspto-grants-2011_03
- 特許番号
- US07915411B2
関連ノート
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