Aminoacetaldehyde dimethyl acetal → 2,2-Dimethoxy-N-(2-oxo-2-((2-phenylethyl)amino)ethyl)ethanaminium chloride

HRID 1045646

반응식

HRID 1045646 반응식
[CH3:1][O:2][CH:3]([O:6][CH3:7])[CH2:4][NH2:5].[Cl:8][CH2:9][C:10]([NH:12][CH2:13][CH2:14][C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1)=[O:11]>C1(C)C=CC=CC=1>[ClH:8].[CH3:1][O:2][CH:3]([O:6][CH3:7])[CH2:4][NH:5][CH2:9][C:10]([NH:12][CH2:13][CH2:14][C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1)=[O:11]

참가 물질

4

반응물 2

HCID 89728Aminoacetaldehyde dimethyl acetalHCID 949212-Chloro-N-phenethyl-acetamide

생성물 1

HCID 462240062,2-Dimethoxy-N-(2-oxo-2-((2-phenylethyl)amino)ethyl)ethanaminium chloride수율 52%

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

Aminoacetaldehyde dimethylacetal (20.05 g, 191 mmol) was added to the solution of 2-chloro-N-phenethyl-acetamide (18.33 g, 92.7 mmol) in toluene (92 ml) and refluxed in 2 hours. After ice-cooling and removal of precipitate by filtration, filtrate was washed with water and dried with magnesium sulfate. The solvents were removed under reduced pressure, and 4N hydrogen chloride in ethyl acetate (18 ml) was added to the residue followed by filtration and wash with ethyl acetate and diethyl ether afforded 2-(2,2-dimethoxy-ethylamino)-N-phenethyl-acetamide hydrochloride (8.77 g, 52%).

후처리

  1. temperaturerefluxed in 2 hours
  2. temperatureAfter ice-cooling
  3. customremoval of precipitate
  4. filtrationby filtration, filtrate
  5. washwas washed with water
  6. dry with materialdried with magnesium sulfate
  7. customThe solvents were removed under reduced pressure, and 4N hydrogen chloride in ethyl acetate (18 ml)
  8. additionwas added to the residue
  9. filtrationfollowed by filtration
  10. washwash with ethyl acetate and diethyl ether

출처 및 근거

ORD 기록
ord-da5f6fad7a7d4445a6d43a7e62205ae6
출처 데이터셋
uspto-grants-2013_10
특허 번호
US08569294B2

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