反应详情

温度

80 °C

To 5 g of phosphorous pentoxide was added 50 ml of methane sulphonic acid. The mixture was heated to 80° C. for 1 hour. The reaction mixture was brought down to 40° C. and 3 g (11.7 mmol) of 2 was added as solid. The mixture was heated at 40° C. for 1 hour and cooled down to room temperature. The reaction mixture was poured into 300 ml of ice/water and extracted with 200 ml of ethyl acetate. The organic layer was washed with 2×150 ml of water, 2×150 ml of saturated NaHCO3 and 100 ml of water. The resulting organic layer was dried (Na2SO4) and concentrated to give 2.6 g (11.7 mmol, 94%) of 3 as off-white powder.

1. customwas brought down to 40° C.
2. temperatureThe mixture was heated at 40° C. for 1 hour
3. temperaturecooled down to room temperature
4. extractionextracted with 200 ml of ethyl acetate
5. washThe organic layer was washed with 2×150 ml of water, 2×150 ml of saturated NaHCO3 and 100 ml of water
6. dry with materialThe resulting organic layer was dried (Na2SO4)
7. concentrationconcentrated