反应详情

Sodium thiomethoxide (0.24 g) was added to a stirred solution of diethyl 3-iodo-3(1-trityl-1,2,4-triazol-3-yl)propane phosphonate (1.0 g, prepared as described in Example 30) in ethanol (10 ml). The mixture was stirred for five hours, allowed to stand overnight, poured into water and extracted with ethyl acetate. The extracts were 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-methylthio-3(1-trityl-1,2,4-triazol-3-yl)propane phosphonate (0.60 g, m.p. 97-98° C.). NMR (CDCl3): δ 1.3(6H,dt), 1.7-1.9(2H,m), 1.9(3H,s), 2.2-2.4(2H,m), 3.9(1H,t), 4.05(4H,m), 7.1(6H,m), 7.3(9H,m), 7.9(1H,s). FAB M/S: MH+ 536.

1. waitto stand overnight
2. extractionextracted with ethyl acetate
3. washThe extracts were washed with brine
4. dry with materialdried over magnesium sulphate
5. customevaporated under reduced pressure
6. customThe residue was chromatographed on silica