反应详情

α-Bromo-p-tolyl cyclobutyl ketone (18.5 g) in dimethylformamide (50 ml) was added during 35 minutes to sodium cyanide (4 g) in dimethylformamide (100 ml) which was cooled below 10° and stirred. The solution was allowed to warm to 20° during 2 hours and poured into water (1 l). The mixture was extracted with ether (3× 200 ml) and the combined extracts were dried over magnesium sulphate, filtered and evaporated. The residue was extracted with light petroleum (b.p. 60°-80°) (7× 250 ml) and the extracts were evaporated to leave an oil which partly crystallised on standing.

1. temperaturewas cooled below 10°
2. temperatureto warm to 20° during 2 hours
3. extractionThe mixture was extracted with ether (3× 200 ml)
4. dry with materialthe combined extracts were dried over magnesium sulphate
5. filtrationfiltered
6. customevaporated
7. extractionThe residue was extracted with light petroleum (b.p. 60°-80°) (7× 250 ml)
8. customthe extracts were evaporated
9. customto leave an oil which
10. custompartly crystallised