反应详情

温度

0 °C

1.15 g (3.37 mmol) of 6-(2,4-dichlorophenyl)-2-(hydroxymethyl)pyrazolo[1,5-a]pyrazin-4(5H)-one (Example 17A) were suspended in 100 ml of dichloromethane, and 1 drop of water was added. 100 ml of 1,2-dimethoxyethane and 9.6 ml of DMF were then added, and the mixture was cooled to 0° C. 7.16 g (16.87 mmol) of Dess-Martin periodinane were added, ice-bath cooling was removed and the mixture was stirred at RT for 15 h. Ethyl acetate and then 200 ml of a 10% strength sodium thiosulfate solution were added to the mixture, and the organic phase was washed with saturated aqueous sodium bicarbonate solution. Drying of the organic phase with sodium sulfate and removal of the solvent under reduced pressure gave 660 mg (57% of theory) of the product as a solid which was reacted without any further purification.

1. temperatureice-bath cooling
2. customwas removed
3. additionEthyl acetate and then 200 ml of a 10% strength sodium thiosulfate solution were added to the mixture
4. washthe organic phase was washed with saturated aqueous sodium bicarbonate solution
5. dry with materialDrying of the organic phase with sodium sulfate and removal of the solvent under reduced pressure