反应详情

Under ice-cooling, pyridine (0.5 mL) and methanesulfonyl chloride (9.9 μL) were sequentially added to a methylene chloride (1 mL) suspension of 2-(2-hydroxy-5-(piperidin-4-yloxy)benzamido)-4-phenylbenzoic acid hydrochloride (0.030 g), followed by stirring at room temperature for 5 hours and 30 minutes. The solvent was evaporated under reduced pressure, and methanol (0.5 mL) and a 2 mol/L aqueous solution of sodium hydroxide (0.5 mL) were added to the residue, followed by stirring at 70° C. for 45 minutes. The reaction mixture was cooled to room temperature, and then 1 mol/L hydrochloric acid (5 mL) was added thereto. The solid substance was collected by filtration and the obtained solid substance was purified by silica gel column chromatography [Kanto Chemical Co., Inc., silica gel 60 (spherical), eluent: chloroform] to obtain 8.0 mg of 2-(2-hydroxy-5-(1-(methylsulfonyl)piperidin-4-yloxy)benzamido)-4-phenylbenzoic acid as a white solid.

1. temperatureUnder ice-cooling
2. customThe solvent was evaporated under reduced pressure, and methanol (0.5 mL)
3. additiona 2 mol/L aqueous solution of sodium hydroxide (0.5 mL) were added to the residue
4. stirringby stirring at 70° C. for 45 minutes
5. temperatureThe reaction mixture was cooled to room temperature
6. addition1 mol/L hydrochloric acid (5 mL) was added
7. filtrationThe solid substance was collected by filtration
8. customthe obtained solid substance was purified by silica gel column chromatography [Kanto Chemical Co., Inc., silica gel 60 (spherical), eluent: chloroform]