反应详情

11.9 g of 10-chloro-10,11-dihydro-2-dimethylsulphamoyldibenzo[b,f]thiepin in 250 ml of chloroform are treated with 20 g of 3-[2-(1-piperazinyl)-ethyl]-2-oxazolidinone and the mixture is heated under reflux for 24 hours. Then the mixture is evaporated under reduced pressure and the residue taken up in ethyl acetate. The organic phase is washed with water, dried over magnesium sulphate and evaporated under reduced pressure. The residue is dissolved in benzene and filtered through a column filled with 100 g of aluminium oxide (activity stage II). The eluate is evaporated and, for the purpose of further purification, chromatographed on 75 g of silicagel (0.2-0.5 mm), elution being effected with a 1:1 mixture of chloroform saturated with concentrated ammonia/carbon tetrachloride. The purified product is recrystallised from ethyl acetate/petroleum ether. There is obtained 3-[2-[4-{10,11-dihydro-2-dimethylsulphamoyl-dibenzo[b,f]thiepin-10-yl}-1-piperazinyl]-ethyl]-2-oxazolidinone which melts at 164°-165° C.

1. temperaturethe mixture is heated
2. temperatureunder reflux for 24 hours
3. customThen the mixture is evaporated under reduced pressure
4. washThe organic phase is washed with water
5. dry with materialdried over magnesium sulphate
6. customevaporated under reduced pressure
7. dissolutionThe residue is dissolved in benzene
8. filtrationfiltered through a column
9. additionfilled with 100 g of aluminium oxide (activity stage II)
10. customThe eluate is evaporated and, for the purpose of further purification
11. customchromatographed on 75 g of silicagel (0.2-0.5 mm), elution
12. additionbeing effected with a 1:1 mixture of chloroform saturated with concentrated ammonia/carbon tetrachloride
13. customThe purified product is recrystallised from ethyl acetate/petroleum ether