反应详情

To chloral (200 ml.) heated to 60°C. under nitrogen was added 11.5 g. of triisopropyldichlorovinyloxyphosphonium chloride (from C-3 above). The clear solution was held overnight under nitrogen at 60°C. and then poured into 400 ml. of dry ether. The oil which first separated became crystalline on standing at room temperature. The solid was collected under nitrogen and recrystallized by dissolution in 80 ml. of dichloromethane and dilution with 400 ml. of dry ether. The crystalline 3/1 chloral/triisopropylphosphine reaction product was collected and dried under dry nitrogen.

1. additionwas added 11.5 g
2. additionpoured into 400 ml
3. customThe oil which first separated
4. customon standing at room temperature
5. customThe solid was collected under nitrogen
6. customrecrystallized by dissolution in 80 ml
7. customThe crystalline 3/1 chloral/triisopropylphosphine reaction product
8. customwas collected
9. customdried under dry nitrogen