反应详情

A mixture of compound 2,6-dichloro-5-iodonicotinonitrile (10 g, 33.4 mmol), cyclopropylboronic acid (3.5 g, 40.1 mmol), K3PO4 (28 g, 133.6 mmol), Cy3P (1 g, 3.3 mmol) and Pd(OAc)2 (0.5 g, 2.2 mmol) in Toluene/H2O (300 mL/15 mL) was stirred under refluxing overnight. The mixture was poured into water and extracted with EtOAc. The separated organics was dried, concentrated and purified by column chromatography (Petroleum ether:EtOAc=10:1) to give compound 2,6-dichloro-5-cyclopropylnicotinonitrile (5 g, 70%). 1H-NMR (400 MHz, CDCl3) δ (ppm) 7.43 (s, 1H), 2.08 (m, 1H), 1.18 (m, 2H), 0.69 (m, 2H)

1. temperatureunder refluxing overnight
2. extractionextracted with EtOAc
3. customThe separated organics was dried
4. concentrationconcentrated
5. custompurified by column chromatography (Petroleum ether:EtOAc=10:1)