Water → HCID 69333344, 화합물

HRID 915062노트

반응식

HRID 915062 반응식
[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

참가 물질

6

반응물 4

HCID 962WaterHCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 69332626HCID 69332626, 화합물

생성물 1

HCID 69333344HCID 69333344, 화합물

시약·촉매·용매 1

HCID 180Acetone용매

반응 조건

온도
27.5 °C

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-c1908a943c3a45ee950509ec22665ea4
출처 데이터셋
uspto-grants-2007_09
특허 번호
US07265120B2

반응 노트

불러오는 중…