反应详情

A solution of 4-(5-trifluoromethyl-tetrazol-1-yl)-phenol (45 mmol) in trifluoroacetic acid (200 ml) and hexamethylenetetramine (186.9 mmol) was heated at 100°, under nitrogen for 16 h. The reaction mixture was quenched with 2N sulphuric acid (250 ml) and extracted with ether (3×250 ml)). The combined organics were dried (Na2SO4) and evaporated to give a dark yellow oil. Purification by FCC (hexane/ether (2:1)) afforded the title compound (8.8 g) as a pale yellow solid. T.I.c. (hexane/ether (2:1)) Rf 0.36

1. customThe reaction mixture was quenched with 2N sulphuric acid (250 ml)
2. extractionextracted with ether (3×250 ml))
3. dry with materialThe combined organics were dried (Na2SO4)
4. customevaporated
5. customto give a dark yellow oil
6. customPurification by FCC (hexane/ether (2:1))