反应详情

A mixture of Intermediate 38 (0.024 g), Intermediate 9 (0.025 g), and 1-methyl-2-pyrrolidinone (1 drop) was subjected was subjected to irradiation in a 600 W microwave oven on full power for 4 mins. The reaction mixture was dissolved in methanol and applied to an ion exchange cartridge (2 g Isolute SCX, pre-conditioned with methanol). Elution with methanol (3 column volumes) followed 10% 0.880 ammonia in methanol (2 column volumes) and evaporation of the first basic fraction in vacuo gave the crude product. Purification by Biotage flash column chromatography on silica gel (8 g cartridge), eluting with 100:8:1 dichloromethane/ethanol/0.880 ammonia, gave the title compound as a white solid (0.025 g). LCMS (System A) Rf 2.85 min Mass Spectrum m/z 479, 481 [MH+]

1. customwas subjected to irradiation in a 600 W microwave oven on full power for 4 mins
2. washElution with methanol (3 column volumes)
3. custom10% 0.880 ammonia in methanol (2 column volumes) and evaporation of the first basic fraction in vacuo
4. customgave the crude product
5. customPurification by Biotage flash column chromatography on silica gel (8 g cartridge)
6. washeluting with 100:8:1 dichloromethane/ethanol/0.880 ammonia