反应详情

Methyl 3-bromo-5-[(dipropylamino)carbonyl]benzoate (Preparation 3) (0.15 g), copper (I) cyanide, and N-methylpyrrolidinone (1 mL) was heated at 150° C. overnight, at which time the mixture was cooled and partitioned between ethyl acetate and aq. HCl (1N). The organic layer was dried (magnesium sulfate), concentrated under reduced pressure, and the residue was chromatographed on silica gel using ethyl acetate-hexane (20/80) to give 0.066 g of the desired product. ms (m+H) 289.2. See also preparation 7 for the preparation of the acid.

1. temperaturewas cooled
2. custompartitioned between ethyl acetate and aq. HCl (1N)
3. dry with materialThe organic layer was dried (magnesium sulfate)
4. concentrationconcentrated under reduced pressure
5. customthe residue was chromatographed on silica gel