反応式
[F:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[C:16]([C:17]3[CH:22]=[CH:21][N:20]=[CH:19][CH:18]=3)=[C:11]3[N:12]=[CH:13][CH:14]=[CH:15][N:10]3[N:9]=2)=[CH:4][CH:3]=1.[C:23](Cl)(=[O:25])[CH3:24].[CH3:27][Mg]Br.C(=O)(O)[O-].[Na+]>O1CCCC1>[C:23]([N:20]1[CH:21]=[CH:22][C:17]([C:16]2[C:8]([C:5]3[CH:6]=[CH:7][C:2]([F:1])=[CH:3][CH:4]=3)=[N:9][N:10]3[CH:15]=[CH:14][CH:13]=[N:12][C:11]=23)=[CH:18][CH:19]1[CH3:27])(=[O:25])[CH3:24]参加物
反応物 4
生成物 1
試薬・触媒・溶媒 1
実験手順
To a solution of 2-(4-fluorophenyl)-3-(pyridin-4-yl)pyrazolo[1,5-a]pyrimidine (480 mg) in dry tetrahydrofuran (15 ml) was added acetyl chloride (0.89 ml) dropwise under ice cooling. The mixture was stirred at ambient temperature for 1 hour and to the mixture was added a solution of methyl magnesium bromide in tetrahydrofuran (1 mole solution, 12.42 ml) under ice cooling. The mixture was stirred at ambient temperature for 2 hours and to the mixture was added an aqueous saturated sodium bicarbonate solution. The separated oil was extracted with dichloromethane and the solution was washed with brine, dried and concentrated in vacuo. The residue was purified by column chromatography on silica gel to give 3-(1-acetyl-l,2-dihydro-2-methylpyridin-4-yl)-2-(4-fluorophenyl)pyrazolo[1,5-a]pyrimidine (327 mg).
後処理
- stirringThe mixture was stirred at ambient temperature for 2 hours and to the mixture
- extractionThe separated oil was extracted with dichloromethane
- washthe solution was washed with brine
- customdried
- concentrationconcentrated in vacuo
- customThe residue was purified by column chromatography on silica gel
出典と根拠
- ORDレコード
- ord-ba5291ff62ad44d885faf03c5746fc87
- 出典データセット
- uspto-grants-1995_12
- 特許番号
- US05478827
関連ノート
読み込み中…