Water → HCID 69333344、化合物

HRID 915062ノート

反応式

HRID 915062 の反応式
[NH2:1][C:2]1[N:3]=[C:4]([C:23]2[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=2)[C:5]([C:13]2[CH:14]=[CH:15][C:16](=[O:22])[N:17]([CH:19]([CH3:21])[CH3:20])[N:18]=2)=[N:6][C:7]=1[C:8]1[CH:9]=[N:10][NH:11][CH:12]=1.[H-].[Na+].I[CH3:32].O>CC(C)=O>[NH2:1][C:2]1[N:3]=[C:4]([C:23]2[CH:24]=[CH:25][CH:26]=[CH:27][CH:28]=2)[C:5]([C:13]2[CH:14]=[CH:15][C:16](=[O:22])[N:17]([CH:19]([CH3:21])[CH3:20])[N:18]=2)=[N:6][C:7]=1[C:8]1[CH:9]=[N:10][N:11]([CH3:32])[CH:12]=1

参加物

6

反応物 4

HCID 962WaterHCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 69332626HCID 69332626、化合物

生成物 1

HCID 69333344HCID 69333344、化合物

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

反応条件

温度
27.5 °C

実験手順

Under nitrogen atmosphere, 6-[5-amino-3-phenyl-6-(1H-pyrazol-4-yl)-2-pyrazinyl]-2-isopropyl-3(2H)-pyridazinone (120 mg) was added to a suspension of NaH (60% in oil) (14.2 mg) and the mixture was stirred at 25-30° C. for 30 minutes. The mixture was cooled in an ice bath and iodomethane (0.1 ml) was added. The mixture was stirred at the same time for 30 minutes and at 20-30° C. for one hour. After addition of water (3.6 ml), a precipitate was collected by filtration and purified by column chromatography on silica gel (EtOAc only) to give a solid. The solid was suspended in acetone and collected by filtration to give 6-[5-amino-6-(1-methyl-1H-pyrazol-4-yl)-3-phenyl-2-pyrazinyl]-2-isopropyl-3(2H)-pyridazinone (70 mg).

後処理

  1. temperatureThe mixture was cooled in an ice bath
  2. stirringThe mixture was stirred at the same time for 30 minutes and at 20-30° C. for one hour
  3. filtrationa precipitate was collected by filtration
  4. custompurified by column chromatography on silica gel (EtOAc only)
  5. customto give a solid
  6. filtrationcollected by filtration

出典と根拠

ORDレコード
ord-c1908a943c3a45ee950509ec22665ea4
出典データセット
uspto-grants-2007_09
特許番号
US07265120B2

反応ノート

読み込み中…