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

HRID 1045646

反応式

HRID 1045646 の反応式
[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]

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-da5f6fad7a7d4445a6d43a7e62205ae6
出典データセット
uspto-grants-2013_10
特許番号
US08569294B2

関連ノート

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