Triethylamine → N-methyl-3-oxo-N-(3-phenyl-2-propene-1-yl)butyramide

HRID 1700338

反応式

HRID 1700338 の反応式
[CH3:1][NH:2][CH2:3][CH:4]=[CH:5][C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1.[CH2:12]=[C:13]1[O:17][C:15](=[O:16])[CH2:14]1.C(N(CC)CC)C.C(=O)([O-])O.[Na+]>C1(C)C=CC=CC=1>[CH3:1][N:2]([CH2:3][CH:4]=[CH:5][C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1)[C:15](=[O:16])[CH2:14][C:13](=[O:17])[CH3:12]

参加物

6

反応物 4

HCID 8471TriethylamineHCID 12661DiketeneHCID 189183N-methyl-3-phenylprop-2-en-1-amineHCID 516892Sodium Bicarbonate

生成物 1

HCID 53834343N-methyl-3-oxo-N-(3-phenyl-2-propene-1-yl)butyramide

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

0.736 g (5.0 mmol) of methyl-(3-phenyl-2-propene-1-yl)amine, 0.386 ml (5.0 mmol) of ketene dimer and 0.07 ml (0.50 mmol) of triethylamine were heated at 70° C. under stirring in 5 ml of toluene overnight. A saturated aqueous sodium hydrogencarbonate solution was added to the reaction mixture. After the extraction with ethyl acetate, the organic layer was dried over anhydrous sodium sulfate. The solvent was evaporated under reduced pressure, and the residue was purified by the thin-layer silica gel chromatography (ethyl acetate) to obtain the title compound.

後処理

  1. extractionAfter the extraction with ethyl acetate
  2. dry with materialthe organic layer was dried over anhydrous sodium sulfate
  3. customThe solvent was evaporated under reduced pressure
  4. customthe residue was purified by the thin-layer silica gel chromatography (ethyl acetate)

出典と根拠

ORDレコード
ord-017d1d1bc74d449d88a6fc94e654953c
出典データセット
uspto-grants-2002_02
特許番号
US06350762B1

関連ノート

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