反应详情

The title compound was prepared in analogy to example 90, from (2-methoxy-[3,4′]bipyridinyl-3′-ylamino)-acetic acid methyl ester and 3-dimethylsulfamoyl-5-trifluoromethyl-benzoic acid (Buttpark Ltd.) after a reaction time of 72 hours. The compound was purified by silica gel chromatography using a MPLC system (CombiFlash Companion, Isco Inc.) eluting with a gradient of n-heptane:EtOAc (100:0 to 20:80). The product-containing fractions were pooled and evaporated and the residue poured on 30 mL 1M aqueous HCl and 30 mL EtOAc. The layers were separated and the aqueous layer was extracted a second time with 30 mL EtOAc. The organic layers were washed twice with 30 mL 1M aqueous HCl followed by 30 mL brine, dried over MgSO4, filtered and concentrated under vacuum. Light yellow solid (30%). MS (ESI): m/z=553.135 [M+H]+.

1. customThe compound was purified by silica gel chromatography
2. washeluting with a gradient of n-heptane:EtOAc (100:0 to 20:80)
3. customevaporated
4. additionthe residue poured on 30 mL 1M aqueous HCl and 30 mL EtOAc
5. customThe layers were separated
6. extractionthe aqueous layer was extracted a second time with 30 mL EtOAc
7. washThe organic layers were washed twice with 30 mL 1M aqueous HCl
8. dry with materialdried over MgSO4
9. filtrationfiltered
10. concentrationconcentrated under vacuum