反应详情

温度

60 °C

To phosphorus oxychloride (0.35 ml, 3.82 mmol) cooled at 0° C. under argon, was added dropwise anhydrous DMF (0.34 ml, 4.46 mmol) and the mixture was stirred for 5 min forming a precipitate. 1.5 ml of DMF were added and stirring was continued at 0° C. for 15 min. To this mixture was added dropwise a solution of the compound of step 2 (0.476 g, 1.27 mmol) in 5 ml of DMF, and the mixture was heated at 60° C. for 1.5 h and then stirred at room temperature overnight. A solution of sodium acetate (0.837 g) in 6.5 ml water was added, the mixture was heated at 50° C. for 1 h, and evaporated to dryness under reduced pressure. The residue was dissolved in EA, the solution was washed with a saturated solution of sodium hydrogencarbonate, water and brine, dried over sodium sulfate, filtered and evaporated to dryness under reduced pressure. The residue was purified by chromatography on silica gel (cyclohexane/EA, 100:0, then 90:10) to give 0.297 g of the title compound.

1. customforming a precipitate
2. stirringstirring
3. waitwas continued at 0° C. for 15 min
4. stirringstirred at room temperature overnight
5. temperaturethe mixture was heated at 50° C. for 1 h
6. customevaporated to dryness under reduced pressure
7. dissolutionThe residue was dissolved in EA
8. washthe solution was washed with a saturated solution of sodium hydrogencarbonate, water and brine
9. dry with materialdried over sodium sulfate
10. filtrationfiltered
11. customevaporated to dryness under reduced pressure
12. customThe residue was purified by chromatography on silica gel (cyclohexane/EA, 100:0