Pyridine → N-methoxy-N-methyl-3-phenylpropanamide

HRID 230880

反応式

HRID 230880 の反応式
Cl.[CH3:2][NH:3][O:4][CH3:5].N1C=CC=CC=1.[C:12]1([CH2:18][CH2:19][C:20](Cl)=[O:21])[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1>ClCCl>[CH3:5][O:4][N:3]([CH3:2])[C:20](=[O:21])[CH2:19][CH2:18][C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1

参加物

5

反応物 3

HCID 1049PyridineHCID 64801Benzenepropanoyl chlorideHCID 81138Methanamine, N-methoxy-, hydrochloride (1:1)

生成物 1

HCID 3785569N-methoxy-N-methyl-3-phenylpropanamide

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a mixture of N,O-dimethylhydroxylamine hydrochloride (1.1 g) and pyridine (1.82 mL) in dichloromethane (50 mL) was added 3-phenylpropionyl chloride (1.52 mL) under ice-cooling, and the mixture was stirred at room temperature for 5 hours. The reaction mixture was concentrated under reduced pressure. To the residue was added 1 mol/L hydrochloric acid, and the mixture was extracted with ethyl acetate. The extract was washed with water and dried over anhydrous magnesium sulfate. The solvent was removed under reduced pressure to give the title compound (1.89 g).

後処理

  1. temperaturecooling
  2. concentrationThe reaction mixture was concentrated under reduced pressure
  3. additionTo the residue was added 1 mol/L hydrochloric acid
  4. extractionthe mixture was extracted with ethyl acetate
  5. washThe extract was washed with water
  6. dry with materialdried over anhydrous magnesium sulfate
  7. customThe solvent was removed under reduced pressure

出典と根拠

ORDレコード
ord-fc82fba548ad4b1f9d02f8cff2363540
出典データセット
uspto-grants-2009_07
特許番号
US07566699B2

関連ノート

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