Tetrahydrofuran → Biphenyl

Temperature

50 °C

4 Grams of polychorinated biphenyl transformer oil (ASKAREL) containing approximately up to 70% PCBs was dissolved in 25 ml of tetrahydrofuran and mixed with 25 g potassium carbonate dissolved in 50 ml water, and 0.5 g of 5% palladium on carbon. The mixture was stirred and warmed to 50° C. To this mixture, while stirring, was added a solution of 10 g sodium hypophosphite monohydrate in 20 ml water dropwise over a period of one hour. Subsequently, an additional 5 g of sodium hypophosphite monohydrate in 10 ml water was added dropwise over a period of 30 minutes. The catalyst was filtered off, the reaction mixture was mixed with 100 ml diethyl ether, the phases separated, the aqueous phase was extracted with 100 ml diethyl ether in 50 ml portions and the organic phases combined. After drying the organic phase with magnesium sulfate, the organic phase was concentrated to yield 0.85 g of biphenyl. A GC analysis made on both the starting material and the reaction product established that all detectable PCB's had been removed.

1. stirringTo this mixture, while stirring
2. filtrationThe catalyst was filtered off
3. additionthe reaction mixture was mixed with 100 ml diethyl ether
4. customthe phases separated
5. extractionthe aqueous phase was extracted with 100 ml diethyl ether in 50 ml portions
6. dry with materialAfter drying the organic phase with magnesium sulfate
7. concentrationthe organic phase was concentrated

ORD record

ord-d85346a6d5a34593899ab62eff5e8f05

Source dataset

uspto-grants-1986_10

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US04618686