反应详情

The crude 4-{4-[5-(3,5-difluoro-benzenesulfonyl)-1-trityl-1H-indazol-3-ylcarbamoyl]-pyrazol-1-yl}-piperidine-1-carboxylic acid tert-butyl ester was dissolved into 15 mL of 1,4-dioxane and added with 3 mL of 4M hydrochloric acid in 1,4-dioxane and stirred at room temperature overnight. Methanol was then added and the mixture stirred for additional 2 hours. The volatiles were removed under reduced pressure, the residue re-dissolved into ethyl acetate, washed with 10% ammonium hydroxide in water, dried over sodium sulfate and evaporated to dryness. The residue was stirred overnight with diethyl ether/methanol 95:5, filtered, washed with diethyl ether/methanol 9:1 then with diethyl ether and dried in oven at 60° C. affording 170 mg of the title compound.

1. stirringthe mixture stirred for additional 2 hours
2. customThe volatiles were removed under reduced pressure
3. dissolutionthe residue re-dissolved into ethyl acetate
4. washwashed with 10% ammonium hydroxide in water
5. dry with materialdried over sodium sulfate
6. customevaporated to dryness
7. stirringThe residue was stirred overnight with diethyl ether/methanol 95:5
8. filtrationfiltered
9. washwashed with diethyl ether/methanol 9:1
10. dry with materialwith diethyl ether and dried in oven at 60° C.