Water → 7-chloro-5-oxo-1-[6-(2-methylbenzoylamino)nicotinoyl]-2,3,4,5-tetrahydro-1H-benzazepine

HRID 1489066ノート

反応式

HRID 1489066 の反応式
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[N:11]([C:12](=[O:20])[C:13]3[CH:18]=[CH:17][C:16]([NH2:19])=[N:15][CH:14]=3)[CH2:10][CH2:9][CH2:8][C:7](=[O:21])[C:6]=2[CH:22]=1.[CH3:23][C:24]1[CH:32]=[CH:31][CH:30]=[CH:29][C:25]=1[C:26](Cl)=[O:27].O>N1C=CC=CC=1>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[N:11]([C:12](=[O:20])[C:13]3[CH:18]=[CH:17][C:16]([NH:19][C:26](=[O:27])[C:25]4[CH:29]=[CH:30][CH:31]=[CH:32][C:24]=4[CH3:23])=[N:15][CH:14]=3)[CH2:10][CH2:9][CH2:8][C:7](=[O:21])[C:6]=2[CH:22]=1

参加物

5

反応物 3

HCID 962WaterHCID 702762-Methylbenzoyl chlorideHCID 229034947-chloro-5-oxo-1-(6-aminonicotinoyl)-2,3,4,5-tetrahydro-1H-benzazepine

生成物 1

HCID 229035137-chloro-5-oxo-1-[6-(2-methylbenzoylamino)nicotinoyl]-2,3,4,5-tetrahydro-1H-benzazepine収率 87.3%

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

To a solution of 7-chloro-5-oxo-1-(6-aminonicotinoyl)-2,3,4,5-tetrahydro-1H-benzazepine (0.25 g) in pyridine (2 ml) is added with stirring 2-methylbenzoyl chloride (0.18 g) under ice-cooling, and the mixture is stirred at room temperature for one hour. To the reaction solution is added water, and the mixture is extracted with ethyl acetate. The extract is washed successively with 0.1N aqueous hydrochloric acid solution and water, and dried over magnesium sulfate. The resultant is evaporated under reduced pressure to remove the solvent, and the residue is purified by silica gel column chromatography to give 7-chloro-5-oxo-1-[6-(2-methylbenzoylamino)nicotinoyl]-2,3,4,5-tetrahydro-1H-benzazepine (0.3 g) as colorless amorphous.

後処理

  1. temperaturecooling
  2. extractionthe mixture is extracted with ethyl acetate
  3. washThe extract is washed successively with 0.1N aqueous hydrochloric acid solution and water
  4. dry with materialdried over magnesium sulfate
  5. customThe resultant is evaporated under reduced pressure
  6. customto remove the solvent
  7. customthe residue is purified by silica gel column chromatography

出典と根拠

ORDレコード
ord-bcfaf860a47946f3ba495a531a831267
出典データセット
uspto-grants-1997_10
特許番号
US05677299

反応ノート

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