反应详情

To a solution of tert-butyl 6-[[2-(4-cyclopropylsulfonylphenyl)-2-(2,4-difluorophenoxy)acetyl]amino]pyridine-3-carboxylate (Example A7; 1.6 g, 2.94 mmole) in DCM (5 mL) was added TFA (7 mL) dropwise at 0° C. Reaction mixture was stirred at rt for 3 hr. TFA was removed invaccuo, residue was neutralised using sat.NaHCO3 solution, extracted with ethyl acetate (3×25 mL) washed with brine, dried over anhydrous sodium sulfate and concentrated. Crude solid was triturated in diisopropyl ether and filtered washed with diisopropyl ether to afford pure product (1.2 g).

1. customReaction mixture
2. customTFA was removed invaccuo, residue
3. extractionNaHCO3 solution, extracted with ethyl acetate (3×25 mL)
4. washwashed with brine
5. dry with materialdried over anhydrous sodium sulfate
6. concentrationconcentrated
7. customCrude solid was triturated in diisopropyl ether
8. filtrationfiltered
9. washwashed with diisopropyl ether