反应详情

While stirring, reflux a solution of 90g of anhydrous piperazine, 52g of 4'-chloro-4-(1-chloroethyl)[1,1']biphenyl and 700 ml of anhydrous benzene for 24 hours. Add 300 ml. of water to the reaction mixture, separate the benzene layer and extract with dilute hydrochloric acid. Separate and filter the acidic aqueous phase, basify the filtrate with dilute sodium hydroxide and extract with methylene chloride. Dry the organic extract, concentrate and triturate the resulting solid residue with petroleum ether. Filter and recrystallize the product from methanol to yield 1-[1-(4'-chloro[1,1']biphenyl-4-yl)ethyl] piperazine m.p. 164°-165° C. The dihydrochloride salt (from methanol as hemihydrate) has a m.p. 263°-264°.

1. additionAdd 300 ml
2. customof water to the reaction mixture, separate the benzene layer
3. extractionextract with dilute hydrochloric acid
4. customSeparate
5. filtrationfilter the acidic aqueous phase
6. extractionextract with methylene chloride
7. customDry the organic extract
8. concentrationconcentrate
9. customtriturate the resulting solid residue with petroleum ether
10. filtrationFilter
11. customrecrystallize the product from methanol