Water → HCID 22903522、化合物

HRID 1489067ノート

反応式

HRID 1489067 の反応式
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[N:11]([C:12](=[O:29])[C:13]3[CH:18]=[CH:17][C:16]([NH:19][C:20](=[O:28])[C:21]4[CH:26]=[CH:25][CH:24]=[CH:23][C:22]=4[CH3:27])=[N:15][CH:14]=3)[CH2:10][CH2:9][CH2:8][C:7](=[O:30])[C:6]=2[CH:31]=1.[BH4-].[Na+].O>CO>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[N:11]([C:12](=[O:29])[C:13]3[CH:18]=[CH:17][C:16]([NH:19][C:20](=[O:28])[C:21]4[CH:26]=[CH:25][CH:24]=[CH:23][C:22]=4[CH3:27])=[N:15][CH:14]=3)[CH2:10][CH2:9][CH2:8][CH:7]([OH:30])[C:6]=2[CH:31]=1

参加物

5

反応物 3

HCID 962WaterHCID 4311764Sodium borohydrideHCID 229035137-chloro-5-oxo-1-[6-(2-methylbenzoylamino)nicotinoyl]-2,3,4,5-tetrahydro-1H-benzazepine

生成物 1

HCID 22903522HCID 22903522、化合物収率 66.4%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

To a solution of 7-chloro-5-oxo-1-[6-(2-methylbenzoylamino)nicotinoyl]-2,3,4,5-tetrahydro-1H-benzazepine (0.3 g) in methanol (5 ml) is added with stirring sodium borohydride (0.05 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 dichloromethane. The extract is washed with 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-hydroxy-1-[6-(2-methylbenzoylamino)nicotinoyl]-2,3,4,5-tetrahydro-1H-benzazepine (0.2 g) as colorless amorphous.

後処理

  1. temperaturecooling
  2. extractionthe mixture is extracted with dichloromethane
  3. washThe extract is washed with 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-1631f34f80df4d4da802dc6455910d1c
出典データセット
uspto-grants-1997_10
特許番号
US05677299

反応ノート

読み込み中…