Carbon tetrabromide → HCID 13246111, compound

In 240 g of methylene chloride were dissolved 12.5 g of carbon tetrabromide, followed by the addition of 19.8 g of triphenylphosphine. The mixture was thoroughly stirred. To this mixed solution were added 5.0 g of the ethyl 2-isopropyl-3-formyl-propionate prepared above and the mixture was stirred at room temperature overnight. Thereafter, the low-boiling fraction was distilled off under reduced pressure and the residue was stirred well with diethyl ether and water. The diethyl ether layer was taken and distilled under reduced pressure to remove the low-boiling fraction. To the residue was added petroleum ether and, after thorough stirring, the petroleum ether solution was taken and further distilled under reduced pressure to remove the low-boiling fraction. The resultant oily residue was purified by distillation under reduced pressure. By the above procedure there were obtained 4.6 g of ethyl α-(3,3-dibromoallyl)isovalerate [yield: 48% based on ethyl 2-isopropyl-3-formyl-propionate].

1. customprepared above and the mixture
2. stirringwas stirred at room temperature overnight
3. distillationThereafter, the low-boiling fraction was distilled off under reduced pressure
4. stirringthe residue was stirred well with diethyl ether and water
5. distillationdistilled under reduced pressure
6. customto remove the low-boiling fraction
7. additionTo the residue was added petroleum ether
8. distillationfurther distilled under reduced pressure
9. customto remove the low-boiling fraction
10. distillationThe resultant oily residue was purified by distillation under reduced pressure

ORD record

ord-89f411e4114c4f71b919fce1480bc24b

Source dataset

uspto-grants-1983_10

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US04409238