反应详情

A mixture of 6.3 g (0.039 m) of N-phenylpiperazine, 4.32 g (0.013 m) of 2-(6,11-dihydro-11-oxodibenz[b,e]oxepin-2-yl)ethanol methanesulfonate of Example 1 and 1.79 g (0.013 m) of K2CO3 in 50 ml of MeOH was refluxed overnight. The reaction mixture was poured into water, extracted with CH2Cl2, dried (Na2SO4), filtered and evaporated to give the crude product (6.5 g). Two recrystallizations from absolute ethanol gave 1.63 g (32%) of crystals of 1-[2-(6,11-dihydro-11-oxodibenz[b,e]oxepin-2-yl)ethyl]-4-phenylpiperazine, m.p. 107°-108° C.

1. temperaturewas refluxed overnight
2. extractionextracted with CH2Cl2
3. dry with materialdried (Na2SO4)
4. filtrationfiltered
5. customevaporated
6. customto give the crude product (6.5 g)
7. customTwo recrystallizations from absolute ethanol