反应详情

To a solution of 2,6-dichloroisonicotinic acid (1 eq.) in DMF (0.05 M) was added sequentially cyclopropylamine (1.05 eq.), Hunig's base (3 eq.) and O-(7-azabenzotriazol-1-yl)-N,N,N′,N′-tetramethyluronium hexafluorophosphate (1.2 eq.). The resulting solution was stirred at RT for 4 h. The reaction was quenched with sat. aq. NH4Cl and extracted with EtOAc. The combined organic extracts were washed with brine, dried over Na2SO4, filtered and the filtrate concentrated in vacuo. Purification of the crude product thus obtained by way of flash chromatography (SiO2, 10:1 (v/v) CH2Cl2:EtOAc) afforded the title compound as a white solid.

1. customThe reaction was quenched with sat. aq. NH4Cl
2. extractionextracted with EtOAc
3. washThe combined organic extracts were washed with brine
4. dry with materialdried over Na2SO4
5. filtrationfiltered
6. concentrationthe filtrate concentrated in vacuo
7. customPurification of the crude product
8. customthus obtained by way of flash chromatography (SiO2, 10:1 (v/v) CH2Cl2:EtOAc)