P-Anisidine → 2-amino-N-(4-methoxy-phenyl)-3-methoxy-benzamide

HRID 617128ノート

反応式

HRID 617128 の反応式
[CH3:1][O:2][C:3]1[C:8]2[NH:9]C(O[C:13](=[O:14])[C:7]=2[CH:6]=[CH:5][CH:4]=1)=O.[CH3:15][O:16][C:17]1[CH:22]=[CH:21][C:20]([NH2:23])=[CH:19][CH:18]=1>C(O)C.CN(C)C1C=CN=CC=1>[NH2:9][C:8]1[C:3]([O:2][CH3:1])=[CH:4][CH:5]=[CH:6][C:7]=1[C:13]([NH:23][C:20]1[CH:21]=[CH:22][C:17]([O:16][CH3:15])=[CH:18][CH:19]=1)=[O:14]

参加物

5

反応物 2

HCID 7732P-AnisidineHCID 105596798-Methoxy-1H-benzo[d][1,3]oxazine-2,4-dione

生成物 1

HCID 181744302-amino-N-(4-methoxy-phenyl)-3-methoxy-benzamide

試薬・触媒・溶媒 2

HCID 142844-(Dimethylamino)pyridine触媒HCID 702Ethanol溶媒

実験手順

To a solution of 27.17 g (0.141 mol) of 8-methoxyisatoic anhydride in 200 mL of ethanol was added a catalytic amount of 4-dimethylaminopyridine and 350 mL of a 1M solution containing 43.0 g (0.350 mol) of p-anisidine. The reaction mixture was stirred and heated under reflux overnight. The reaction flask was then chilled on ice. The precipitate that formed was collected by vacuum filtration and amounted to 34.7 g. An analytical sample (mp 168-169° C.) was obtained by recrystallization from ethanol.

後処理

  1. temperatureheated
  2. temperatureunder reflux overnight
  3. temperatureThe reaction flask was then chilled on ice
  4. customThe precipitate that formed
  5. filtrationwas collected by vacuum filtration
  6. customAn analytical sample (mp 168-169° C.) was obtained by recrystallization from ethanol

出典と根拠

ORDレコード
ord-f72bda8dcd30406794af07be74c69540
出典データセット
uspto-grants-1999_09
特許番号
US05948775

反応ノート

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