反应详情

Intermediate 30 (0.041 g) was added to a stirred solution of Intermediate 29 (0.110 g) in N,N-dimethylformamide (2 ml) at 22° C., and N,N-diisopropylethylamine (0.052 ml) was added. After stirring for 20 h, the mixture was applied in two equal portions to ion exchange cartridges (10 g Isolute SCX pre conditioned with methanol). Elution with methanol (3 column volumes) followed by 10% 0.880 ammonia in methanol (2 column volumes) and evaporation of the first basic fractions in vacuo gave the crude product. Purification by Biotage flash 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, (0.0828 g).

1. washElution with methanol (3 column volumes)
2. customfollowed by 10% 0.880 ammonia in methanol (2 column volumes) and evaporation of the first basic fractions in vacuo
3. customgave the crude product
4. customPurification by Biotage flash chromatography on silica gel (8 g cartridge)
5. washeluting with 100:8:1 dichloromethane/ethanol/0.880 ammonia