反应详情

To a solution of 8.0 g (0.045 mol) of 73 in 125 ml of toluene, 10 g (0.045 mol) of P4S10 was added. The suspension was refluxed for 4 h and left at room temperature overnight. The mixture was poured into ice water followed by basification with ammonia. The two-phase system was stirred with charcoal and filtered. The toluene phase was separated and the aqueous phase extracted with 2×100 ml of toluene. The combined organic phases were dried over MgSO4 and evaporated in vacuo leaving a heavy, yellow oil, 88. Yield: 2.3 g (0.013 mol, 29%).

1. temperatureThe suspension was refluxed for 4 h
2. filtrationfiltered
3. customThe toluene phase was separated
4. extractionthe aqueous phase extracted with 2×100 ml of toluene
5. dry with materialThe combined organic phases were dried over MgSO4
6. customevaporated in vacuo
7. customleaving a heavy, yellow oil, 88