反应详情

To a stirred solution of 2-aminopyridine-N-oxide in chloroform at 0° C. was added dropwise a solution of DMAD (1 eq.) in chloroform. After addition the cooling bath was removed and stirring was continued for 1 hour. A further 0.2 eq. of DMAD was added and stirring continued for 1 hour. The solution was filtered over a silica gel plug. After elution with EtOAc/PE (4:6), the product was eluted with MeOH/EtOAc. The combined MeOH/EtOAc-phases were concentrated to dryness. The title compound was obtained as a brown oil, which was used without further purification.

1. additionAfter addition the cooling bath
2. customwas removed
3. stirringstirring
4. waitcontinued for 1 hour
5. filtrationThe solution was filtered over a silica gel plug
6. washAfter elution with EtOAc/PE (4:6)
7. washthe product was eluted with MeOH/EtOAc
8. concentrationThe combined MeOH/EtOAc-phases were concentrated to dryness