反应详情

A mixture of methyl 2-chloro-4-nitrobenzoate (2 g, 9.3 mmol), CuCN (3.3 g, 37.2 mmol), and Pd(PPh3)4 (1.075 g, 0.93 mmol) was suspended in DMF (15 mL) and then subjected to microwave irradiation at 150° C. for 4 hours. After the mixture was concentrated under reduced pressure, the residue was partitioned between ethyl acetate and water. The organic layer was dried over Na2SO4, filtered, and the filtrate was evaporated to dryness under reduced pressure. The crude material was purified by column chromatography (20% EA/PE) to afford 0.9 g of title compound. LC-MS: m/z 207.1 (M+H)+.

1. customirradiation at 150° C. for 4 hours
2. concentrationAfter the mixture was concentrated under reduced pressure
3. customthe residue was partitioned between ethyl acetate and water
4. dry with materialThe organic layer was dried over Na2SO4
5. filtrationfiltered
6. customthe filtrate was evaporated to dryness under reduced pressure
7. customThe crude material was purified by column chromatography (20% EA/PE)