反应详情

0.8 G. of 10-chloro-10,11-dihydro-2,8-dimethyl-dibenz[b,f]oxepin and 0.58 g. of 1-methyl-piperazine are dissolved in 4 ml. of chloroform and heated at reflux for 21 hours. Then, the chloroform is evaporated in vacuo. The residue is partitioned between benzene and aqueous sodium carbonate solution. The benzene solution is extracted with dilute hydrochloric acid. The hydrochloric acid extract is made alkaline with sodium carbonate and extracted with benzene. Thereafter, the benzene extract is washed several times with water, dried over sodium sulfate, evaporated in vacuo, and there is obtained 1-[10,11-dihydro-2,8-dimethyl-dibenz[ b,f]oxepin-10-yl] -4-methyl-piperazine, the dihydrochloride of which melts at 197°- 198° C. (with decomposition).

1. temperatureat reflux for 21 hours
2. customThen, the chloroform is evaporated in vacuo
3. customThe residue is partitioned between benzene and aqueous sodium carbonate solution
4. extractionThe benzene solution is extracted with dilute hydrochloric acid
5. extractionThe hydrochloric acid extract
6. extractionextracted with benzene
7. extractionThereafter, the benzene extract
8. washis washed several times with water
9. dry with materialdried over sodium sulfate
10. customevaporated in vacuo