反应详情

温度

170 °C

A mixture of 5-bromo-4-methyl-pyridin-2-ylamine (500 mg, 2.67 mmol), CuCN (478 mg, 5.34 mmol) and DMA (2 mL) was stirred under nitrogen for 20 h at 170° C. The reaction mixture was cooled and added to 50 mL of a 20% aqueous solution of ethane-1,2-diamine. The layers were separated and the aqueous layer was extracted 3× with EtOAc. The combined organics were washed with water followed by brine and dried over MgSO4. Concentration in vacuo afforded compound 851A (309 mg, 87%) as a white solid.

1. temperatureThe reaction mixture was cooled
2. customThe layers were separated
3. extractionthe aqueous layer was extracted 3× with EtOAc
4. washThe combined organics were washed with water
5. dry with materialdried over MgSO4
6. concentrationConcentration in vacuo