反应详情

0.28 g of 5-(3,4-dimethoxyphenyl)-2-{1-[(5-hydroxy-2-methylphenyl)carbonyl]piperidin-4-yl}-4,4-dimethyl-2,4-dihydro-3H-pyrazol-3-one (compound described in example 85) and 0.25 g potassium carbonate are suspended in 5 ml of acetonitrile. 0.31 g of 2-iodopropane is added and the reaction mixture is heated to reflux under a blanket of nitrogen for about 16 h until the reaction is completed according to TLC analysis. The solvent is evaporated under reduced pressure, and the remaining residue is taken up in EA. The organic phase is washed with water, twice with 1 M aqueous sodium hydroxide solution and with brine, dried over MgSO4, and the solvent is removed under reduced pressure. Purification of the resulting crude product by crystallization from diethyl ether yields the title compound.

1. temperaturethe reaction mixture is heated
2. temperatureto reflux under a blanket of nitrogen for about 16 h until the reaction
3. customThe solvent is evaporated under reduced pressure
4. washThe organic phase is washed with water, twice with 1 M aqueous sodium hydroxide solution and with brine
5. dry with materialdried over MgSO4
6. customthe solvent is removed under reduced pressure
7. customPurification of the resulting crude product
8. customby crystallization from diethyl ether