反应详情

温度

80 °C

394 mg (1 mmol) of 3-(3-amino-4-trifluoromethoxyphenyl)-5,5-dimethyl-1-pyridin-4-ylmethylimidazolidine-2,4-dione were dissolved in 1 ml of DMF, 166 mg (1.2 mmol) of potassium carbonate and 413 mg (1.3 mmol) of 1-(diphenylmethyl)-3-azetidine methanesulphonate were added, and the mixture was stirred at 80° C. for 5 h. For workup, the mixture was added to ice-water, extracted with CH2C12, dried and concentrated. The remaining residue was purified by means of preparative HPLC (RP18, acetonitrile/water, 0.1% TFA). The intermediate obtained in this way was dissolved in 3 ml of methanol, admixed with 10 mg of 5% Pd/C and 50 mg (0.8 mmol) of ammonium formate, and heated under reflux for 2 h. The residue remaining after filtration and evaporation was purified by means of preparative HPLC (RP18, acetonitrile/water, 0.1% TFA).

1. extractionextracted with CH2C12
2. customdried
3. concentrationconcentrated
4. customThe remaining residue was purified by means of preparative HPLC (RP18, acetonitrile/water, 0.1% TFA)
5. customThe intermediate obtained in this way
6. temperatureheated
7. temperatureunder reflux for 2 h
8. filtrationafter filtration and evaporation
9. customwas purified by means of preparative HPLC (RP18, acetonitrile/water, 0.1% TFA)