反応式
[CH3:1][CH:2]([N:4]1[C:8]([C:9]([NH:11][C:12]2[C:13]3[C:17]([CH:18]=[C:19](B4OC(C)(C)CC(C)(C)O4)[CH:20]=2)=[N:16][N:15](C2CCCCO2)[CH:14]=3)=[O:10])=[CH:7][CH:6]=[N:5]1)[CH3:3].P([O-])([O-])([O-])=O.[K+].[K+].[K+].Br[C:46]1[CH:54]=[CH:53][CH:52]=[C:51]2[C:47]=1[CH2:48][C:49](=[O:55])[NH:50]2.O1CCOCC1>O>[CH3:3][CH:2]([N:4]1[C:8]([C:9]([NH:11][C:12]2[CH:20]=[C:19]([C:46]3[CH:54]=[CH:53][CH:52]=[C:51]4[C:47]=3[CH2:48][C:49](=[O:55])[NH:50]4)[CH:18]=[C:17]3[C:13]=2[CH:14]=[N:15][NH:16]3)=[O:10])=[CH:7][CH:6]=[N:5]1)[CH3:1]参加物
反応物 4
生成物 1
試薬・触媒・溶媒 1
反応条件
- 温度
- 120 °C
実験手順
A microwave vial was charged with 1-(1-methylethyl)-N-[2-(tetrahydro-2H-pyran-2-yl)-6-(4,4,6,6-tetramethyl-1,3,2-dioxaborinan-2-yl)-2H-indazol-4-yl]-1H-pyrazole-5-carboxamide (70 mg), Solvias catalyst (8 mg), tripotassium phosphate (90 mg) and 4-bromo-1,3-dihydro-2H-indol-2-one (available from Apollo, 33 mg), 1,4-dioxane (0.5 ml) and water (0.1 ml). The reaction was heated under microwave irradiation for a total of 30 min at 120° C.). Further tripotassium phosphate (60 mg) and Solvias catalyst (8 mg) were added and the reaction was heated under microwave irradiation for 10 min at 120° C. The reaction was passed through a silica cartridge, dried, then extracted with DCM and water before drying the DCM under a stream of nitrogen. The residue was purified as follows:
後処理
- temperaturethe reaction was heated under microwave irradiation for 10 min at 120° C
- customdried
- extractionextracted with DCM and water
- dry with materialbefore drying the DCM under a stream of nitrogen
- customThe residue was purified
出典と根拠
- ORDレコード
- ord-24350e1fd4df42aab3394d4225181213
- 出典データセット
- uspto-grants-2014_02
- 特許番号
- US08658635B2
関連ノート
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