反应详情

To a solution of methyl 6-[3-[4-chloro-3-[[(methoxycarbonyl)amino]methyl]phenyl]-1H-pyrazol-1-yl]-2H-1-benzopyran-3-carboxylate (i.e. the product of Step C) (100 mg, 0.22 mmol) in 1:1 tetrahydrofuran/water was added NaOH (35 mg 0.85 mmol) and the reaction mixture was stirred at ambient temperature for 6 hrs. After TLC analysis (50% ethyl acetate/pet ether) showed completion of reaction, the organic solvent was concentrated. The resultant aqueous solution was cooled to 0° C., acidified with 1N HCl and extracted three times with ethyl acetate. The combined the organic phases were washed with water, brine, dried over Na2SO4. The solvent was concentrated under vacuum to give compound number 24, a compound of the present invention, (70 mg, 73% yield) as solid.

1. customcompletion of reaction
2. concentrationthe organic solvent was concentrated
3. temperatureThe resultant aqueous solution was cooled to 0° C.
4. extractionextracted three times with ethyl acetate
5. washwere washed with water, brine
6. dry with materialdried over Na2SO4
7. concentrationThe solvent was concentrated under vacuum
8. customto give compound number 24