ethyl 4-((3S,5R)-3,5-diMethylpiperazin-1-yl)benzoate synthesis

Yield:234082-05-4 92.8%

Reaction Conditions:

in (methylsulfinyl)methane at 120; for 28 h;Inert atmosphere;

Steps:

1.4 Step 4: Preparation of 4 - ((3R, 5S) -3,5-dimethylpiperazin-1-yl) benzoate

0.44 ml of ethyl 4-fluorobenzoate was dissolved in 8 ml of dimethylsulfoxide, 1.370 g of (2S, 6R) -dimethylpiperazine was added,The temperature was raised to 120 ° C under argon protection, and the mixture was heated for 28 hours. After heating, the reaction solution was diluted with 40 ml of water,Ethyl ester extraction, organic phase after the merger with saturated aqueous sodium chloride solution washed five times, anhydrous sodium sulfate drying, filtration concentrated, residualThe residue was chromatographed (dichloromethane: methanol = 99: 1-97: 3, V / V) to give 0.730 g of a brown oil in a yield of 92.8%.

References:

CN106146493,2016,A Location in patent:Paragraph 0172; 0173; 0174; 0175