反应详情

A solution of diethyl 3-bromo-3(1-trityl-1,2,4-triazol-3-yl)propane phosphonate (1.0 g, prepared as described in Example 29) and sodium iodide (1.30 g) in acetone (15 ml) was allowed to stand for twenty hours at room temperature in the absence of light. It was then filtered through Hyflo Super-Cel, evaporated under reduced pressure and the residue partitioned between ethyl acetate and water. The organic layer was washed with brine, dried over magnesium sulphate and evaporated under reduced pressure. The residue was chromatographed on silica, using dichloromethane-ethanol (49:1) as eluant, to give diethyl 3-iodo-3(1-trityl-1,2,4-triazol-3-yl)propane phosphonate (0.85 g, m.p. 98-100° C.). NMR (CDCl3): δ 1.3(6H,t), 1.7-1.9(2H,m), 2.5-2.6(2H,m), 4.05(4H,m), 5.3(1H,t), 7.1(6H,m), 7.3(9H,m), 7.9(1H,s). M/S: M+ 615.

1. waitto stand for twenty hours at room temperature in the absence of light
2. filtrationIt was then filtered through Hyflo Super-Cel
3. customevaporated under reduced pressure
4. customthe residue partitioned between ethyl acetate and water
5. washThe organic layer was washed with brine
6. dry with materialdried over magnesium sulphate
7. customevaporated under reduced pressure
8. customThe residue was chromatographed on silica