反应详情

温度

60 °C

45 mg (0.11 mmol) of Lawesson reagent (2,4-bis[4-methoxyphenyl] 1,3-dithia-2,4-diphosphetane 2,4-disulphide) were added to a solution of 10 mg (0.20 mmol) of 1-(morpholin-4-ylcarbonyl)-5-[4-(trifluoromethyl)phenyl]piperidine-3-carboxamide (Example 52A) in 1 ml of dioxane, and the reaction mixture was stirred at 60° C. for 30 minutes and then at room temperature for 3 h. After addition of saturated aqueous sodium bicarbonate solution and removal of the dioxane, the residue was extracted with ethyl acetate. The organic phase was washed with a saturated aqueous sodium bicarbonate solution, dried over magnesium sulphate, filtered and concentrated under reduced pressure. This gave 43 mg (100% of theory) of crude product, which was reacted without any further purification steps.

1. waitat room temperature for 3 h
2. extractionthe residue was extracted with ethyl acetate
3. washThe organic phase was washed with a saturated aqueous sodium bicarbonate solution
4. dry with materialdried over magnesium sulphate
5. filtrationfiltered
6. concentrationconcentrated under reduced pressure
7. customThis gave 43 mg (100% of theory) of crude product, which was reacted without any further purification steps