反应详情

温度

90 °C

A mixture containing crude 3-(2-hydroxymethyl-4-iodophenoxy)-3-methyl-2-butanone (0.84 g, 0.00252 mol) and triphenylphosphine hydrobromide (0.86 g, 0.00252 mol) in acetonitrile (5 ml) was heated at 90° C. for 2.5 hours. After evaporation of the solvent, the crude solid product was washed with ether and dissolved in ethanol (3 ml). Hot isopropyl ether (8 ml) was added until a light precipitate formed, and the solution was left at room temperature overnight. The crystalline product was recovered by filtration to yield 0.77 g (50%) of 2-(1-methyl-2-oxo-propyloxy)-5-iodobenzyltriphenylphosphonium bromide, m.p. 230° C.

1. customAfter evaporation of the solvent
2. washthe crude solid product was washed with ether
3. dissolutiondissolved in ethanol (3 ml)
4. additionHot isopropyl ether (8 ml) was added until a light precipitate
5. customformed
6. filtrationThe crystalline product was recovered by filtration