反应详情

温度

160 °C

2-Amino-N-methyl-5-(5-methylhexahydropyrrolo[3,4-c]pyrrole-2(1H)-yl)benzamide (Intermediate 8A) (100 mg, 0.36 mmol) was dissolved in triethoxymethane (1 mL) and sealed in a microwave vial. Heated at 160° C. for 10 minutes. Reaction allowed to cool to room temperature and lithium hydroxide solution added (0.5 mL, 1M in methanol) and reaction stirred overnight. Organic layer loaded onto a 1 g SCX cartridge. The crude material was purified by SCX, and the solvent removed under reduced pressure. The crude material was then re-dissolved in methanol (1 mL) and purified by preparative-HPLC. Purified sample was free-based using 500 mg SCX cartridge to afford 3-methyl-6-(5-methylhexahydropyrrolo[3,4-c]pyrrole-2(1H)-yl)quinazolin-4(3H)-one (56 mg, 0.2 mmol).

1. customsealed in a microwave vial
2. customReaction
3. temperatureto cool to room temperature
4. customThe crude material was purified by SCX
5. customthe solvent removed under reduced pressure
6. dissolutionThe crude material was then re-dissolved in methanol (1 mL)
7. custompurified by preparative-HPLC
8. customPurified sample