反应详情

10 Grams (39.7 mM) of 6-(4-chlorobutyryl)-3,4-dihydrocarbostyril was dissolved in 300 ml of benzene, then to this solution was added 7.4 g (120 mM) of ethylene glycol and 300 mg of p-toluenesulfonic acid, and the whole mixture was refluxed by heating under dehydrating in Dean-Stark extractor for 6 hours. The reaction mixture was cooled and neutralized with an aqueous solution saturated with sodium hyfrogen carbonate, then extracted with chloroform. The chloroform extract was washed with water then dried with anhydrous magnesium sulfate, then concentrated by removing the solvent by evaporation. The residue thus obtained was purified by means of a silicagel column chromatography (eluent: chloroform:methanol=40:1) to yield 10.5 g of 6-(1-ethylenedioxy-4-chlorobutyl)-3,4-dihydrocarbostyril.

1. temperaturethe whole mixture was refluxed
2. temperatureby heating under dehydrating in Dean-Stark extractor for 6 hours
3. temperatureThe reaction mixture was cooled
4. extractionextracted with chloroform
5. extractionThe chloroform extract
6. washwas washed with water
7. dry with materialthen dried with anhydrous magnesium sulfate
8. concentrationconcentrated
9. customby removing the solvent
10. customby evaporation
11. customThe residue thus obtained
12. customwas purified by means of a silicagel column chromatography (eluent: chloroform:methanol=40:1)