反応式
[NH:1]1[C:9]2[C:4](=[C:5]([C:10]3[CH:11]=[C:12]([NH2:19])[C:13]4[CH:14]=[N:15][NH:16][C:17]=4[CH:18]=3)[CH:6]=[CH:7][CH:8]=2)[CH:3]=[CH:2]1.[C:20]1(=O)[C:24]2[CH:25]=[CH:26][CH:27]=[CH:28][C:23]=2[C:22](=[O:29])[O:21]1.CN(C=O)C>ClCCl>[NH:1]1[C:9]2[C:4](=[C:5]([C:10]3[CH:18]=[C:17]4[C:13]([CH:14]=[N:15][NH:16]4)=[C:12]([N:19]4[C:20](=[O:21])[C:24]5[C:23](=[CH:28][CH:27]=[CH:26][CH:25]=5)[C:22]4=[O:29])[CH:11]=3)[CH:6]=[CH:7][CH:8]=2)[CH:3]=[CH:2]1参加物
反応条件
- 温度
- 150 °C
実験手順
A mixture of 6-(1H-indol-4-yl)-1H-indazol-4-amine (500 mg, 2.014 mmol), 2-benzofuran-1,3-dione (298 mg, 2.014 mmol) and DMF (2.5 ml) was placed in a Biotage vial (2-5 ml) equipped with a magnetic stirrer bar. The vial was placed in a Biotage Initiator microwave and heated at 150° C. for 30 min then again at 150° C. for a further 15 min. The reaction mixture was evaporated to dryness to give a brown oil which was dissolved in dichloromethane and applied to a 100 g silica SPE cartridge. The cartridge was eluted on a Flashmaster (II) instrument using a gradient of 0-100% ethyl acetate in cyclohexane over 40 min followed by 0-20% methanol in cyclohexane over 15 min. Appropriate fractions were combined and evaporated to give the title compound (481 mg) as a pale yellow foam.
後処理
- customequipped with a magnetic stirrer bar
- customThe reaction mixture was evaporated to dryness
- customto give a brown oil which
- washThe cartridge was eluted on a Flashmaster (II) instrument
- customover 40 min
- waitfollowed by 0-20% methanol in cyclohexane over 15 min
- customevaporated
出典と根拠
- ORDレコード
- ord-86134a09b94647c7bd01f6a44bdf76c2
- 出典データセット
- uspto-grants-2013_09
- 特許番号
- US08536169B2
関連ノート
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