Triethylamine → Butyrylamino-acetic acid methyl ester

HRID 607136

反応式

HRID 607136 の反応式
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

  1. temperaturecooled to 0° under a nitrogen atmosphere
  2. washThe reaction was washed with saturated aqueous sodium bicarbonate (50 mL), water (50 mL) and brine
  3. dry with materialThe organic phase was dried over anhydrous sodium sulfate
  4. filtrationfiltered
  5. 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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