1-((2-(4-chlorophenyl)-5,5-diMethylcyclohex-1-enyl)Methyl)piperazine synthesis

Yield:1228838-29-6 100%

Reaction Conditions:

with trifluoroacetic acid in dichloromethane; for 1 h;

Steps:

5.4

Step 4 Synthesis of 1 -[2-(4-chloro-phenyl)-5,5-dimethyl-cyclohex-l -enylmethyl]-piperazineTo 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 OfNaHCO₃ was added to adjust the pH to ~8-9 and the mixture was extracted with dichloromethane (x2). The combined extracts were washed with brine, dried (Na₂SO₄), filtered and concentrated under reduced pressure to give l-[2-(4-chloro-phenyl)-5,5-dimethyl-cyclohex-l-enylmethyl]-piperazine (0.76 g, 100%). HPLC-MS 319, 321 [M+l]⁺.

References:

WO2010/67067,2010,A1 Location in patent:Page/Page column 42