反应详情

温度

90 °C

1.88 ml of formalin and 1.07 g of methylfuran were added to a mixture of 4.43 g (15.7 mmol) of 4-(4-methylsulfonylaminobenzoyl)piperidine in free form obtained in Example 17, 1.57 ml of glacial acetic acid and 10 ml of water and the obtained mixture was stirred at 90° C. for 2 h. After cooling, the mixture was neutralized with a 20% aqueous sodium hydroxide solution and extracted with dichloromethane. The organic layer was washed with water and a saturated aqueous common salt solution, dried over magnesium sulfate and concentrated. The solid residue was recrystallized from ethanol/methanol to obtain 4.16 g (yield: 70%) of the intended compound.

1. temperatureAfter cooling
2. extractionextracted with dichloromethane
3. washThe organic layer was washed with water
4. dry with materiala saturated aqueous common salt solution, dried over magnesium sulfate
5. concentrationconcentrated
6. customThe solid residue was recrystallized from ethanol/methanol