反応式
[Cl:1][C:2]1[CH:3]=[N:4][N:5]([CH3:10])[C:6]=1[C:7](O)=[O:8].ClC(N(C)C)=C(C)C.[NH:19]1[C:27]2[C:22](=[C:23]([C:28]3[CH:29]=[C:30]([NH2:37])[C:31]4[CH:32]=[N:33][NH:34][C:35]=4[CH:36]=3)[CH:24]=[CH:25][CH:26]=2)[CH:21]=[CH:20]1.C(N(CC)CC)C>C(Cl)Cl>[Cl:1][C:2]1[CH:3]=[N:4][N:5]([CH3:10])[C:6]=1[C:7]([NH:37][C:30]1[CH:29]=[C:28]([C:23]2[CH:24]=[CH:25][CH:26]=[C:27]3[C:22]=2[CH:21]=[CH:20][NH:19]3)[CH:36]=[C:35]2[C:31]=1[CH:32]=[N:33][NH:34]2)=[O:8]参加物
6
反応物 4
生成物 1
試薬・触媒・溶媒 1
反応条件
- 温度
- 20 °C
実験手順
A solution of 4-chloro-1-methyl-1H-pyrazole-5-carboxylic acid (available from Fluorochem) (50 mg) in dry DCM (10 ml) was treated with 1-chloro-N,N,2-trimethyl-1-propen-1-amine (0.041 ml) (available from Acros) and allowed to stir at 20° C. for 10 min when a solution of 6-(1H-indol-4-yl)-1H-indazol-4-amine (77 mg) and triethylamine (0.043 ml) in DCM (5 ml) was added and the mixture stirred at 20° C. for 18 h. The mixture was poured onto an aminopropyl SPE cartridge (1 g) and allowed to stand for 2 h, then the mixture was eluted with methanol (5 ml) and blown to dryness under a stream of nitrogen. The crude product was purified by mass directed preparative HPLC (Method A) to give the title compound as a white solid (15 mg).
後処理
- additionwas added
- waitto stand for 2 h
- washthe mixture was eluted with methanol (5 ml)
- customThe crude product was purified by mass
出典と根拠
- ORDレコード
- ord-2b1ae7de5fd848489294a21c25a2a9c3
- 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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