反应详情

A mixture of 3-[4-(5-bromo-3-methylpyrid-2-yl)butyl]-6-(pyrid-3-ylmethyl)-3H-1,2,3-triazolo[5,4-b]-pyridine (0.6 g) and polyphosphoric acid (ca. 6 g) was heated with stirring at 190°-200° C. for 40 minutes. The cooled residue was dissolved in aqueous ammonium hydroxide to give a solution of ca. pH 8 and extracted with chloroform (4 x 30 ml). The combined chloroform extracts were dried over magnesium sulphate, concentrated in vacuo and the residue was chromatographed on silica eluted with 7.5% v/v methanol in chloroform and then recrystallised under ether to give the title compound (0.12 g), m.p. 164°-166° C.

1. temperaturewas heated
2. customto give a solution of ca. pH 8
3. extractionextracted with chloroform (4 x 30 ml)
4. dry with materialThe combined chloroform extracts were dried over magnesium sulphate
5. concentrationconcentrated in vacuo
6. customthe residue was chromatographed on silica
7. washeluted with 7.5% v/v methanol in chloroform
8. customrecrystallised under ether