反应详情

Phosphorus pentasulfide (56.5 g) and Na2CO3 (13.7 g) were mixed together in 400 mL of THF for ~30 min. To this solution, a solution of the product of Step 1 (17.32 g) in 100 mL of THF was added and the mixture was stirred at room temperature overnight. 2M NaOH (500 mL) was added and the mixture was stirred at room temperature for 2 hr. The product was extracted in EtOAc, washed with brine, dried over Na2SO4, and purified by flash chromatography on silica with EtOAc: toluene 20:80; yield: 12.07 g, (83%).

1. stirringthe mixture was stirred at room temperature for 2 hr
2. extractionThe product was extracted in EtOAc
3. washwashed with brine
4. dry with materialdried over Na2SO4
5. custompurified by flash chromatography on silica with EtOAc: toluene 20:80