反应详情

Potassium tert-butylate (2.75 g, 23.7 mmol) was provided in abs. ether (50 mL) in argon and mixed with butyl-triphenyl phosphonium bromide (9.45 g, 23.7 mmol). The batch was heated for 30 min to 40° C. 4-dimethylamino-4-phenyl cyclohexanone (5.00 g, 23.0 mmol) dissolved in abs. THF (50 mL) was then added carefully in drops (exothermic reaction). The batch was heated for 6.5 h to 50° C. and stirred overnight at room temperature. The batch was then concentrated in a vacuum until dry, taken up in dioxan (20 mL) and mixed with HO/dioxan (5 mL). A precipitate separated out during this. This was filtered off, washed with ether (10 mL), then basified with 2N NaOH and extracted with dichloromethane (2×40 mL). The organic phase was dried over Na2SO4, filtered and concentrated in a vacuum until dry.

1. temperatureThe batch was heated for 30 min to 40° C
2. temperatureThe batch was heated for 6.5 h to 50° C.
3. concentrationThe batch was then concentrated in a vacuum
4. customuntil dry
5. additionmixed with HO/dioxan (5 mL)
6. customA precipitate separated out during this
7. filtrationThis was filtered off
8. washwashed with ether (10 mL)
9. extractionextracted with dichloromethane (2×40 mL)
10. dry with materialThe organic phase was dried over Na2SO4
11. filtrationfiltered
12. concentrationconcentrated in a vacuum
13. customuntil dry