反应详情

4.9 Grams of 1-methyl-7-(3-chloropropoxy)-3,4-dihydrocarbostyril, 4.2 g of 4-benzylpiperidine and 3 g of triethylamine were mixed with 60 ml of dimethylformamide. The mixture was heated at 70°-80° C. for 8 hours. After the reaction was completed, the reaction mixture was concentrated under a reduced pressure to dryness. To the residue thus obtained was added 5%-sodium hydrogencarbonate aqueous solution and extracted with chloroform. The chloroform layer was washed with water and dried, then chloroform was removed by distillation. The residue thus obtained was dissolved in 30 ml of acetone, and under stirring condition a 5%-oxalic acid acetone solution was added thereto to make pH 4.5 then was allowed to stand. Precipitates thus formed were obtained by filtration, washed with acetone, then recrystallized from ethanol-ether to obtain 7.9 g (yield: 86%) of 1-methyl-7-[3-(4-benzyl-1-piperidyl)propoxy]-3,4-dihydrocarbostyril monooxalate as in the form of colorless powder. Melting point: 175°-177° C.

1. temperatureThe mixture was heated at 70°-80° C. for 8 hours
2. concentrationthe reaction mixture was concentrated under a reduced pressure to dryness
3. customTo the residue thus obtained
4. extractionextracted with chloroform
5. washThe chloroform layer was washed with water
6. customdried
7. customchloroform was removed by distillation
8. customThe residue thus obtained
9. additionwas added
10. customPrecipitates thus
11. customformed
12. customwere obtained by filtration
13. washwashed with acetone
14. customrecrystallized from ethanol-ether