反应详情

Ammonium isothiocyanate (7.726 g, 0.1015 mol) was added to a solution of 2,6-dichloro-4-pyridinecarbonyl chloride (17.8 g, 0.0846 mol) in acetone (300 ml). The mixture was stirred for 30 minutes and subsequently 2,3,4-trifluorobenzenamine hydrochloric acid (.HCl) was added slowly. The reaction mixture was stirred at room temperature for 2 hours and was then quenched with H2O (100 ml). The mixture was extracted with CH2Cl2 (3×80 ml) and the combined organic layers were dried (MgSO4), filtered and the solvent was evaporated in vacuo. The residue was purified by flash chromatography (eluent: heptane/EtOAc from 80/20 to 50/50). The desired fractions were collected and the solvent was evaporated in vacuo. Yield: 22.2 g of intermediate D9 (69%).

1. stirringThe reaction mixture was stirred at room temperature for 2 hours
2. customwas then quenched with H2O (100 ml)
3. extractionThe mixture was extracted with CH2Cl2 (3×80 ml)
4. dry with materialthe combined organic layers were dried (MgSO4)
5. filtrationfiltered
6. customthe solvent was evaporated in vacuo
7. customThe residue was purified by flash chromatography (eluent: heptane/EtOAc from 80/20 to 50/50)
8. customThe desired fractions were collected
9. customthe solvent was evaporated in vacuo