反应详情

1 g (2.66 mmol) of 5-(2,4-difluorophenyl)-3-iodo-salicylic acid was mixed with 0.738 g (4.01 mmol) of pentafluorophenol in 20 ml of acetonitrile. 10 ml of N,N-diisopropylcarbodiimide was added at 0° C. and it was stirred continuously. 0.634 g of ammonium bicarbonate was dissolved in water. Consumption of the starting product was confirmed by HPLC and the crude was diluted with water and extracted with dichloromethane. The organic phase was dried over magnesium sulphate and purified on a silica gel column, using chloroform and methanol as eluents, in increasing polarity beginning with a proportion (v/v) of (40:1) up to (10:1).

1. customConsumption of the starting product
2. additionthe crude was diluted with water
3. extractionextracted with dichloromethane
4. dry with materialThe organic phase was dried over magnesium sulphate
5. custompurified on a silica gel column
6. temperaturein increasing polarity beginning with a proportion (v/v) of (40:1) up to (10:1)