反应详情

[2-Amino-6-(2-methoxy-ethoxy)-3-nitro-pyridin-4-yl]-benzyl-carbamic acid ethyl ester (118 mg) was dissolved in ethanol (5 ml) and 10% Pd on carbon (15 mg) added. The reaction was stirred under a hydrogen atmosphere (50 psi) for 1 h at RT. The reaction mixture was then filtered through a Celite pad and evaporated. The crude was dissolved in glacial acetic acid (2 ml) and transferred to a microwave vial (Biotage, 0.5-2.0 ml). The vial was sealed and heated under microwave irradiation at 100° C. for 5 minutes. The resultant brown mixture was evaporated then solid loaded on silica and columned on Isco Companion on a silica column (4 g, Redisep), eluting with EtOAc:heptane, increasing the gradient linearly from 60:40 to 100% EtOAc over 8 column volumes (CVs) then isocratic at 100% EtOAc for 8 CVs. The desired fractions were combined and evaporated to provide the title compound as a white solid (50 mg).

1. filtrationThe reaction mixture was then filtered through a Celite pad
2. customevaporated
3. dissolutionThe crude was dissolved in glacial acetic acid (2 ml)
4. customThe vial was sealed
5. temperatureheated under microwave irradiation at 100° C. for 5 minutes
6. customThe resultant brown mixture was evaporated
7. washeluting with EtOAc
8. temperatureheptane, increasing the gradient linearly from 60
9. customevaporated