反应详情

4-Chlorobutryl chloride (388.0 g) was added at 40° to a solution of technical grade 8-aminoquinoline (3396.5 g) and triethylamine (278.3 g) in dimethoxyethane (2 l). After stirring overnight at ambient temperature the solids were filtered off. The filtrate was concentrated prior to additon of 13% potassium tert-butoxide in tert-butanol (2486 g) at 25°-30°. After two hours the mixture was neutralized with dilute hydrochloric acid. The slurry obtained by partial removal of the solvent was extracted three times with methylene chloride. The combined extracts were washed with water, dried over magnesium sulphate, filtered and concentrated. Ether (1 l) was added while cooling to 0°. Filtration, followed by vacuum-drying afforded 1-(8-quinolyl)-2-pyrrolidinone.

1. filtrationwere filtered off
2. concentrationThe filtrate was concentrated
3. customat 25°-30°
4. waitAfter two hours the mixture was neutralized with dilute hydrochloric acid
5. customThe slurry obtained by partial removal of the solvent
6. extractionwas extracted three times with methylene chloride
7. washThe combined extracts were washed with water
8. dry with materialdried over magnesium sulphate
9. filtrationfiltered
10. concentrationconcentrated
11. additionEther (1 l) was added
12. temperaturewhile cooling to 0°
13. filtrationFiltration
14. customby vacuum-drying