反应详情

A solution of N-(2,6-dihydroxyphenyl)-3-cyclopentyloxy-4-methoxyphenyl-acetamide (2.10 g) and pyridinium p-toluene-sulphonate (532 mg) in xylene (100 ml) was refluxed, under nitrogen, overnight. The reaction mixture was cooled to room temperature, diluted with water (100 ml), and extracted with dichloromethane (3×75 ml). The combined organic extracts were washed with water (3×100 ml), brine (100 ml), dried (CaSO4) and evaporated in-vacuo to yield a pale brown solid. The solid was purified by flash chromatography (SiO2; dichloromethane;methanol (50:1)) to yield the title compound (1.027 g, 51%) as a white solid (mp 172-181° C.).

1. extractionextracted with dichloromethane (3×75 ml)
2. washThe combined organic extracts were washed with water (3×100 ml), brine (100 ml)
3. dry with materialdried (CaSO4)
4. customevaporated in-vacuo
5. customto yield a pale brown solid
6. customThe solid was purified by flash chromatography (SiO2; dichloromethane;methanol (50:1))