反应详情

55 ml of a 32% NaOH solution is added in drops at room temperature to a mixture that consists of 11.0 g (20.1 mmol) of 1,3,5-triiodo-2,4,6-trishydroxymethylbenzene, 55.5 g (0.6 mol) of epichlorohydrin and 1.1 g (3.2 mmol) of tetrabutylammonium hydrogen sulfate within 1 hour, and then it is stirred for 12 hours. It is mixed with 150 ml of water and extracted twice with 200 ml each of toluene. The combined organic phases are dried on sodium sulfate, the solvent is evaporated to the dry state and chromatographed on silica gel (mobile solvent:hexane/ethyl acetate 10:1). The fractions that contain the product are combined and concentrated by evaporation.

1. extractionextracted twice with 200 ml each of toluene
2. customThe combined organic phases are dried on sodium sulfate
3. customthe solvent is evaporated to the dry state
4. customchromatographed on silica gel (mobile solvent:hexane/ethyl acetate 10:1)
5. concentrationconcentrated by evaporation