반응 #70531

반응 방정식

6-(1H-indol-4-yl)-1H-indazol-4-amine

2-benzofuran-1,3-dione

DMF

→

title compound

수율 63.1%

2-[6-(1H-Indol-4-yl)-1H-indazol-4-yl]-1H-isoindole-1,3(2H)-dione

수율 63.1%

용매

dichloromethane

반응 조건

후처리

1. 1
   기타equipped with a magnetic stirrer bar
2. 2
   기타The reaction mixture was evaporated to dryness
3. 3
   기타to give a brown oil which
4. 4
   세척The cartridge was eluted on a Flashmaster (II) instrument
5. 5
   기타over 40 min
6. 6
   workup.WAITfollowed by 0-20% methanol in cyclohexane over 15 min
7. 7
   기타evaporated

실험 절차

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.

출처