反应详情

温度

22 °C

To a solution of 1,1′-carbonyldiimidazole (0.041 g) in dichloromethane (2 ml) at 0° C. was added dropwise a solution of Intermediate 41 (0.079 g) in dichloromethane (2 ml). The mixture was stirred at 0° C. for 1 h and at 22° C. for 1 h, re-cooled to approximately 0° C. and a solution of 4-aminomethylbenzamide (0.041 g) in a 1:1 mixture of dichloromethane and N,N-dimethylformiamide (4 ml) was added dropwise. The mixture was stirred at 0° C. for 1 h and at 22° C. for 1 h, and applied in two equal portions to ion exchange cartridges (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 basic fractions in vacuo gave the crude product. Purification by Biotage flash chromatography on a silica gel cartridge (89), eluting with 150:8:1 dichloromethane/ethanol/0.880 ammonia, gave the title compound as a white solid (0.0186 g).

1. temperaturere-cooled to approximately 0° C.
2. additionwas added dropwise
3. stirringThe mixture was stirred at 0° C. for 1 h and at 22° C. for 1 h
4. washElution with methanol (3 column volumes)
5. custom10% 0.880 ammonia in methanol (2 column volumes) and evaporation of the basic fractions in vacuo
6. customgave the crude product
7. customPurification by Biotage flash chromatography on a silica gel cartridge (89)
8. washeluting with 150:8:1 dichloromethane/ethanol/0.880 ammonia