反应详情

N,N-Diisopropylethylamine (0.109 mL, 0.625 mmol) was added to a solution of 3-(4-{[4-[5-fluoro-2-(methyloxy)phenyl]-2-hydroxy-4-methyl-2-(trifluoromethyl)pentyl]amino}-6-methyl-1H-indazol-1-yl)benzoic acid (70 mg, 0.125 mmol) and HATU (47.5 mg, 0.125 mmol) in DMF (2.5 mL) and the solution stirred at room temperature for 5 min. Glycine hydrochloride (34.6 mg, 0.313 mmol) was added and the mixture stirred at room temperature overnight and then partitioned between 2M HCl (50 mL) and ethyl acetate (50 mL). The organic layer was separated, washed with aqueous sodium bicarbonate (50 ml), dried over anhydrous sodium sulphate and evaporated to give crude product which was purified by mass directed autopreparation (System B) to give the title compound (62.5 mg).

1. stirringthe mixture stirred at room temperature overnight
2. custompartitioned between 2M HCl (50 mL) and ethyl acetate (50 mL)
3. customThe organic layer was separated
4. washwashed with aqueous sodium bicarbonate (50 ml)
5. dry with materialdried over anhydrous sodium sulphate
6. customevaporated
7. customto give crude product which
8. customwas purified by mass