反应详情

2-Amino-5-bromobenzoic acid methyl ester (4.6 g, 20 mmol) and copper (I) cyanide (3.6 g, 40 mmol) were heated at 200° C. in N-methylpyrrolidinone (20 ml) for 4 h. After cooling to room temperature, the solution was diluted with water, extracted with ethyl acetate, the aqueous extract acidified with 2N hydrochloric acid and filtered. The organic layer was separated, dried over magnesium sulphate and evaporated. The residue was purified by flash column chromatography on silica eluting with 50% ethyl acetate in hexane to yield the title compound as a colourless oil (1.0 g). MS (+El) m/z 176 [M+].

1. extractionextracted with ethyl acetate
2. extractionthe aqueous extract
3. filtrationfiltered
4. customThe organic layer was separated
5. dry with materialdried over magnesium sulphate
6. customevaporated
7. customThe residue was purified by flash column chromatography on silica eluting with 50% ethyl acetate in hexane