反应详情

温度

160 °C

In a microwave safe flask, 3-cyclopropyl-3-(4-(3-iodo-7-(1-methyl-1H-pyrazol-4-yl)imidazo[1,2-c]pyrimidin-5-yl)-1H-pyrazol-1-yl)propanenitrile (22.4 mg, 0.0463 mmol) and cyanocopper (4.56 mg, 0.0509 mmol) were suspended in DMF (463 μL, 0.0463 mmol). The reaction mixture was heated at 160° C. for 1 hour. The reaction mixture was cooled and diluted in EtOAc and 10% NH4OH (10 mL). The mixture was separated and the aqueous layer extracted with EtOAc. The combined organic layers were washed with brine, dried with MgSO4, filtered and concentrated in vacuo. Purification using preparative TLC in 15% MeOH/EtOAc afforded 5-(1-(2-cyano-1-cyclopropylethyl)-1H-pyrazol-4-yl)-7-(1-methyl-1H-pyrazol-4-yl)imidazo[1,2-c]pyrimidine-3-carbonitrile (11.0 mg, 62.0% yield). MS (apci) m/z=384.4 (M+H).

1. temperatureThe reaction mixture was cooled
2. customThe mixture was separated
3. extractionthe aqueous layer extracted with EtOAc
4. washThe combined organic layers were washed with brine
5. dry with materialdried with MgSO4
6. filtrationfiltered
7. concentrationconcentrated in vacuo
8. customPurification