Hydrochloride methanol → Hydrochloric Acid

Participants

Reaction Conditions

Reaction Steps

[Method 1] (R)-6-(2-(tert-butoxycarbonyl(2-(3-(N-(tert -butoxycarbonyl)methylsulfonamido)phenyl)-2-(triethylsilyloxy)ethyl)amino)ethoxy)-1-(tetrahydro -2H -pyran-2-yl)-3-trifluoromethylindazole (85.6 mg) that can be produced by the method described in Reference Example 30 or the like, was dissolved in a 10% hydrogen chloride-methanol solution (1.5 mL; manufactured by Tokyo Chemical Industry Co., Ltd.), and the solution was purged with nitrogen and stirred for 39 hours at 50° C. The reaction solution was cooled to room temperature, and then nitrogen gas was blown into the reaction solution to evaporate the solvent. The operation of adding diethyl ether to the residue, and blowing nitrogen gas into the reaction solution to evaporate the solvent, was repeated three times. The resulting residue was purified by HPLC, and then the purified product was dissolved in methanol (2 mL). A 10% hydrogen chloride-methanol solution (0.2 mL; manufactured by Tokyo Chemical Industry Co., Ltd.) was added to the solution, and nitrogen gas was blown into the solution to evaporate the solvent. The residue was dissolved in water (1 mL), and the solution was freeze-dried. Thus, the title compound was obtained in the form of hydrochloride (31 mg).

Provenance & Evidence