反应详情

A mixture of 4-fluoro-2-hydroxy-N-methyl-benzamide (0.3 g, 1.77 mmol) in formaldehyde (37% aq. soln) (2 mL) and formic acid (2 mL) was refluxed for 1 hour then poured onto ice. The mixture was neutralised with sodium carbonate and extracted into chloroform (3×30 mL). The combined organics were dried (MgSO4), and reduced in vacuo to give a white solid which was chromatographed on silica, eluting with 10-50% ethyl acetate in isohexane to give the desired compound as a white solid (0.24 g).

1. temperaturewas refluxed for 1 hour
2. additionthen poured onto ice
3. extractionextracted into chloroform (3×30 mL)
4. dry with materialThe combined organics were dried (MgSO4)
5. customto give a white solid which
6. customwas chromatographed on silica
7. washeluting with 10-50% ethyl acetate in isohexane