反应详情

A stirred solution of 1,2,4-triazole (0.15 g) in dry N,N-dimethylformamide (10 ml) was treated, under nitrogen, with sodium hydride (0.075 g, 60% in oil) and 15-Crown-5 (0.02 g). After ten minutes, the stirred mixture was treated with diethyl 3-bromo-3(1-trityl-1,2,4-triazol-3-yl)propane phosphonate (1.0 g, prepared as described in Example 29). After a further three hours, it was poured into water and extracted with ethyl acetate. The extracts were washed with brine, dried over magnesium sulphate and evaporated under reduced pressure, finally at 0.01 mm. The residue was chromatographed on silica, using dichloromethane-ethanol (19:1) as eluant, to give diethyl 3(1,2,4-triazol-1-yl)-3(1-trityl-1,2,4-triazol-3-yl)propane phosphonate (0.39 g) as a colourless oil. NMR (CDCl3): δ1.2(6H,dt), 1.7-1.8(2H,m), 2.6-2.8(2H,m), 4.05(4H,m), 5.7(1H,t), 7.1(6H,m), 7.3(9H,m), 7.95(2H,2xs), 8.25(1H,s). M/S: M+ 556.

1. waitAfter ten minutes
2. extractionextracted with ethyl acetate
3. washThe extracts were washed with brine
4. dry with materialdried over magnesium sulphate
5. customevaporated under reduced pressure, finally at 0.01 mm
6. customThe residue was chromatographed on silica