反应详情

温度

80 °C

A suspension of 0.20 g (0.6 mmol) 7-hydroxy-6-(3-hydroxy-3-phenyl-propyl)-3-methoxymethyl-2-methyl-3H-benzoimidazole-5-carboxylic acid dimethylamide in 2 ml 85% ortho-phosphorlc acid was heated to 80° C. After 90 min stirring, the reaction was cooled to room temperature, poured into ice/water and neutralized with 10M sodium hydroxide. The water layer was extracted with dichloromethane, the organic layers were dried over magnesium sulphate and concentrated in vacuo. The residue was crystallized from ethyl acetate/petroleum ether to afford 130 mg (59%) of the title compound as a beige powder. m.p. 213°-215° C.

1. temperaturethe reaction was cooled to room temperature
2. extractionThe water layer was extracted with dichloromethane
3. dry with materialthe organic layers were dried over magnesium sulphate
4. concentrationconcentrated in vacuo
5. customThe residue was crystallized from ethyl acetate/petroleum ether