反応式
[CH2:1]([O:8][C:9]1[CH:14]=[C:13]([F:15])[CH:12]=[CH:11][C:10]=1[C:16](=[O:31])[CH2:17][N:18]1[CH2:23][CH2:22][N:21]([C:24]([O:26][C:27]([CH3:30])([CH3:29])[CH3:28])=[O:25])[CH2:20][CH2:19]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1>COC(OC)N(C)C>[C:27]([O:26][C:24]([N:21]1[CH2:22][CH2:23][N:18]([C:17]([C:16](=[O:31])[C:10]2[CH:11]=[CH:12][C:13]([F:15])=[CH:14][C:9]=2[O:8][CH2:1][C:2]2[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=2)=[CH:17][N:18]([CH3:23])[CH3:19])[CH2:19][CH2:20]1)=[O:25])([CH3:28])([CH3:30])[CH3:29]参加物
実験手順
A solution of 2′-(benzyloxy)-2-[4-(tert-butoxycarbonyl)piperazin-1-yl]4′-fluoroacetophenone (270 mg, 0.63 mmol) in dimethylformamide dimethylacetal (1.5 mL) was heated in a sealed microwave tube at 200° C. for 15 minutes. A white precipitate formed. The mixture was evaporated to dryness in vacuo to give crude 4-[1-(2-benzyloxy-4-fluoro-benzoyl)-2-dimethylamino-vinyl]-piperazine-1-carboxylic acid tert-butyl ester. Ethanol (2 mL) and hydrazine hydrate (2.0 mL) were added and the mixture heated in a sealed microwave tube at 120° C. for 30 minutes. The crude mixture was loaded onto a dry pre-packed silica cartridge and dried overnight. The product was eluted with 2:1 hexane:EtOAc to give 4-[3-(2-benzyloxy-4-fluoro-phenyl)-1H-pyrazol-4-yl]-piperazine-1-carboxylic acid tert-butyl ester (95 mg, 33%) as a yellow gum; LCMS retention time 2.75 min, M+H+ 453.4.
後処理
- customA white precipitate formed
- customThe mixture was evaporated to dryness in vacuo
出典と根拠
- ORDレコード
- ord-adb7828d57c84442aeeef43bceeeeb3a
- 出典データセット
- uspto-grants-2009_11
- 特許番号
- US07612201B2
関連ノート
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