反应详情

A solution of 2-methylphenylmagnesium bromide is prepared from 2.7 g of magnesium, 19 g of 1-bromo-2-methylbenzene and 100 ml of ether. A mixture of 5.04 g of 5-chloroisatin and 100 ml of THF is cooled in an ice bath under an argon atmosphere and the solution of magnesium compound prepared above is added slowly. After stirring for 4 hours, water is added and the solvents are evaporated off under vacuum. The residue is extracted with AcOEt, the precipitate formed is filtered off and the organic phase of the filtrate is dried over magnesium sulfate and evaporated under vacuum. The residue obtained, combined with the precipitate previously filtered off, is crystallized from MeOH to give 4.8 g of the expected product.

1. temperatureis cooled in an ice bath under an argon atmosphere
2. additionabove is added slowly
3. customthe solvents are evaporated off under vacuum
4. extractionThe residue is extracted with AcOEt
5. customthe precipitate formed
6. filtrationis filtered off
7. dry with materialthe organic phase of the filtrate is dried over magnesium sulfate
8. customevaporated under vacuum
9. customThe residue obtained
10. filtrationpreviously filtered off
11. customis crystallized from MeOH