反应详情

To a suspension of 3.0 g (8.86 mmol) 10-hydroxy-5,6,8,9-tetrahydro-1,4,7,10a-tetraaza-cyclohepta[f]indene-7-carboxylic acid benzyl ester in 6 mL toluene was added 7 mL (74.06 mmol) of phosphorus oxychloride and 1.28 mL (7.35 mmol) of DIPEA, and the reaction was heated at reflux for 40 minutes. The mixture was cooled to room temperature and poured into ice. The aqueous phase was extracted with DCM (3×20 mL) and the combined organic layers were dried over MgSO4. After filtration and evaporation of the solvent the product was purified by column chromatography (silica, heptane/EtOAc 9:1 to 7:3).

1. temperaturethe reaction was heated
2. temperatureat reflux for 40 minutes
3. additionpoured into ice
4. extractionThe aqueous phase was extracted with DCM (3×20 mL)
5. dry with materialthe combined organic layers were dried over MgSO4
6. filtrationAfter filtration and evaporation of the solvent the product
7. customwas purified by column chromatography (silica, heptane/EtOAc 9:1 to 7:3)