反应详情

According to Scheme 5 Step 2: The title compound was prepared from 5-(4-methoxyphenyl)-(1H)-pyridin-2-one (1 eq, 0.50 mmol, 0.10 g, Example 7 Step 1) and 5-(chloromethyl)-2-(trifluoromethyl)pyridine (1.5 eq, 0.74 mmol, 0.15 g) according to the procedure described for Example 1 Step 2. Reaction conditions: 6 hours at 70° C. and 48 hours at room temperature. The crude product was purified by silica gel chromatography (AIT Flashsmart prepacked column 10 g SiO2, CH2Cl2/AcOEt 90/10). The purified oil was dissolved in Et2O and HCl (4M in dioxane) was added. The resulting precipitate was filtered, dried to afford 5-(4-methoxyphenyl)-1-((6-(trifluoromethyl)pyridin-3-yl)methyl)pyridin-2(1H)-one hydrochloride (83 μmol, 30 mg, 17%) as a white solid.

1. customReaction conditions
2. custom6 hours
3. customat 70° C.
4. custom48 hours
5. customat room temperature
6. customThe crude product was purified by silica gel chromatography (AIT Flashsmart prepacked column 10 g SiO2, CH2Cl2/AcOEt 90/10)
7. dissolutionThe purified oil was dissolved in Et2O
8. additionHCl (4M in dioxane) was added
9. filtrationThe resulting precipitate was filtered
10. customdried