反应详情

温度

70 °C

A mixture of 63.0 mg of 4-[2-Benzyl-6-[(3R,4R)-3-hydroxy-4-methoxypyrrolidin-1-yl]-3-pyridyl]-1-methyl-4-piperidinol (Example 3) and 1.5 ml of 1 M acetic acid solution of hydrogen chloride was stirred at 70° C. for 9 hours. The reaction mixture was neutralized with an aqueous sodium hydrogen carbonate solution and extracted with ethyl acetate. The organic layer was washed with water and brine, dried over anhydrous magnesium sulfate, and the solvent was removed. To the residue were added 50 mg of potassium carbonate and 1 ml of methanol, followed by stirring at room temperature for 1 hour. NH-silica gel was added to the reaction mixture and the solvent was removed. It was purified by NH-silica gel column chromatography with 5% methanol/ethyl acetate, to give 10.2 mg of the title compound.

1. extractionextracted with ethyl acetate
2. washThe organic layer was washed with water and brine
3. dry with materialdried over anhydrous magnesium sulfate
4. customthe solvent was removed
5. additionTo the residue were added 50 mg of potassium carbonate and 1 ml of methanol
6. stirringby stirring at room temperature for 1 hour
7. additionNH-silica gel was added to the reaction mixture
8. customthe solvent was removed
9. customIt was purified by NH-silica gel column chromatography with 5% methanol/ethyl acetate