反应详情

温度

90 °C

Add zinc dust (1.18 g) to a suspension of 2,3-dichloro-5-trifluoromethyl-pyridine (2.0 g, 9.30 mmol) in 80:20 water and acetic acid (5 mL) and stir at 90° C. for 1 h. Add more zinc dust (1g) and stir at 90° C. for an additional 15 min. Cool the reaction mixture to room temperature, filter, and wash with dichloromethane. Carefully concentrate and purify the residue by silica gel chromatography, eluting with 100:0 to 0:100 hexane:dichloromethane, to obtain the title compound as a volatile oil (0.120g, 7%).

1. stirringstir at 90° C. for an additional 15 min
2. temperatureCool the reaction mixture to room temperature
3. filtrationfilter
4. washwash with dichloromethane
5. concentrationCarefully concentrate
6. custompurify the residue by silica gel chromatography
7. washeluting with 100:0 to 0:100 hexane