反应详情

3-chloro-2-(7-chloro-1,3-benzodioxol-5-yl)-4,4,4-trifluoro-but-2-enenitrile (20.2 g, 65.4 mmol) was dissolved in ethanol (200 mL) and treated with pyrimidin-2-yl-hydrazine (7.20 g, 65.4 mmol) and triethylamine (6.60 g, 65.4 mmol). The reaction mixture was heated to reflux for 10 h. The solvent was removed in vacuo, to the residue was added water, extracted with EtOAc, then the organic layer was combined, washed with water and brine, dried, filtered and concentrated to give crude product. The crude product was washed with DCM to give the title compound (11.0 g; 44%).

1. temperatureThe reaction mixture was heated
2. temperatureto reflux for 10 h
3. customThe solvent was removed in vacuo, to the residue
4. additionwas added water
5. extractionextracted with EtOAc
6. washwashed with water and brine
7. customdried
8. filtrationfiltered
9. concentrationconcentrated
10. customto give crude product
11. washThe crude product was washed with DCM