反应详情

A solution of lithium di-isopropylamide (2M in heptane, 25 ml) was added to a solution of 2,6-dichlorobenzonitrile (8.6 g) in THF while maintaining the temperature below -70° C. The mixture was stirred for 1.5 hours then poured onto solid carbon dioxide. It was stirred for 1 hour then diluted with ether. Water was added and the mixture was acidified to pH1. It was extracted with ether, washed with water, dried (MgSO4) and filtered. The filtrate was evaporated to dryness to give 3-cyano-2,4-dichlorobenzoic acid (9.4 g) as a white solid mp 230°-232° C.

1. temperaturewhile maintaining the temperature below -70° C
2. stirringIt was stirred for 1 hour
3. extractionIt was extracted with ether
4. washwashed with water
5. dry with materialdried (MgSO4)
6. filtrationfiltered
7. customThe filtrate was evaporated to dryness