反应详情

To a solution of 4-[2-(4-chloro-phenyl)-5,5-dimethyl-cyclohex-1-enylmethyl]-piperazine-1-carboxylic acid tert-butyl ester (1.0 g, 2.39 mmol) in dichloromethane (20 ml) was added TFA (5 ml). The reaction was stirred for 1 h and then concentrated under reduced pressure. A saturated solution of NaHCO3 was added to adjust the pH to ˜8-9 and the mixture was extracted with dichloromethane (×2). The combined extracts were washed with brine, dried (Na2SO4), filtered and concentrated under reduced pressure to give 1-[2-(4-chloro-phenyl)-5,5-dimethyl-cyclohex-1-enylmethyl]-piperazine (0.76 g, 100%). HPLC-MS 319, 321 [M+1]+.

1. concentrationconcentrated under reduced pressure
2. additionA saturated solution of NaHCO3 was added
3. extractionthe mixture was extracted with dichloromethane (×2)
4. washThe combined extracts were washed with brine
5. dry with materialdried (Na2SO4)
6. filtrationfiltered
7. concentrationconcentrated under reduced pressure