반응 #65471

반응 방정식

1-(2-cyclopropylphenyl)piperazine

3-bromo-N-methyl-N-(triphenylmethyl)propanamine

potassium carbonate

→

3-[4-(2-cyclopropylphenyl)piperazin-1-yl]-N-methyl-N-(tri-phenylmethyl)propanamine

수율 18.2%

용매

dimethylformamide

반응 조건

후처리

1. 1
   기타equipped with a reflux condenser
2. 2
   기타The solvent is evaporated under reduced pressure
3. 3
   기타the organic phase is separated
4. 4
   세척washed with water
5. 5
   건조dried over sodium sulphate
6. 6
   기타the solvent is evaporated under reduced pressure

실험 절차

9.0 g (0. 0444 mol) of 1-(2-cyclopropylphenyl)piperazine, 200 ml of dimethylformamide, 17.5 g (0.0444 mol) of 3-bromo-N-methyl-N-(triphenylmethyl)propanamine and 9 g of potassium carbonate are introduced into a 500 ml round-bottomed flask equipped with a reflux condenser and placed under nitrogen, and the mixture is heated three times for 6 h at 96° C. The solvent is evaporated under reduced pressure, the residue is taken up with water and dichloromethane, the organic phase is separated, washed with water, dried over sodium sulphate and the solvent is evaporated under reduced pressure. There are obtained 4.17 g of 3-[4-(2-cyclopropylphenyl)piperazin-1-yl]-N-methyl-N-(tri-phenylmethyl)propanamine in the form of an oil which is dissolved in 200 ml of methanol, a stream of gaseous hydrochloric acid is passed therein for 10 min, the mixture is concentrated, allowed to stand for 2 days and the precipitate is separated by filtration. 2.94 g of compound are obtained.

출처