Triethylamine → HCID 15337836、化合物
反応式
Cl.[CH2:2]([NH2:6])/[CH:3]=[CH:4]/[CH3:5].Br[CH2:8][C:9]([O:11][CH3:12])=[O:10].CCN(CC)CC>C(#N)C>[CH2:2]([NH:6][CH2:8][C:9]([O:11][CH3:12])=[O:10])/[CH:3]=[CH:4]/[CH3:5]参加物
5
実験手順
A suspension of (E)-2-buten-1-amine HCl (5.37 g, 49.9 mmol) (Chem. Ber. 117, 1250(1984) in acetonitrile (100 mL) was treated with methyl bromoacetate (4.72 mL, 49.9 mmol) and Et3N (14.0 mL, 99.8 mmol) and stirred at room temperature for I hour. The suspension was then heated at reflux overnight. Solution occurred at reflux temperature. After cooling, the precipitated Et3N.HCl was filtered off and the solvent removed under reduced pressure leaving 5.0 g of the crude product. Chromatography on silica gel, eluting with CHCl3/MeOH (98/2) gave 1.41 g (19.8% yield) of the pure product as an oil.
後処理
- temperatureThe suspension was then heated
- temperatureat reflux overnight
- temperatureat reflux temperature
- temperatureAfter cooling
- filtrationthe precipitated Et3N.HCl was filtered off
- customthe solvent removed under reduced pressure
- customleaving 5.0 g of the crude product
- washChromatography on silica gel, eluting with CHCl3/MeOH (98/2)
出典と根拠
- ORDレコード
- ord-b48ead47966248b78789211493f77817
- 出典データセット
- uspto-grants-2002_04
- 特許番号
- US06369034B1
反応ノート
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