Triethylamine → HCID 15337836, 화합물
반응식
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]참가 물질
5
실험 절차
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.
후처리
- 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)
출처 및 근거
- ORD 기록
- ord-b48ead47966248b78789211493f77817
- 출처 데이터셋
- uspto-grants-2002_04
- 특허 번호
- US06369034B1
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