1,3-Dibromopropane → HCID 20061406, compound

A mixture of 4.16 g of 2,6-dichloro-4-nitrophenol, 40.4 g of 1,3-dibromopropane, 2.76 g of potassium carbonate and 2.46 g of potassium t-butoxide was heated under reflux for 4 hours in 50 ml of methyl ethyl ketone. The reaction mixture was allowed to cool down and insoluble matters were filtered off. The filtrate was concentrated under reduced pressure. The residue was dissolved in chloroform. The thus-prepared chloroform solution was washed with water, and the chloroform was then distilled off. The residue was purified by chromatography on a silica gel column (eluent: chloroform/hexane=4/1, by volume) to obtain 6.24 g of 1-bromo-3-(2,6-dichloro-4-nitrophenyloxy)propane. This compound was employed in the next reaction without any further purification.

1. temperaturewas heated
2. temperatureto cool down
3. filtrationinsoluble matters were filtered off
4. concentrationThe filtrate was concentrated under reduced pressure
5. dissolutionThe residue was dissolved in chloroform
6. washThe thus-prepared chloroform solution was washed with water
7. distillationthe chloroform was then distilled off
8. customThe residue was purified by chromatography on a silica gel column (eluent: chloroform/hexane=4/1, by volume)

ORD record

ord-0d2a0a8c0bf840bba81e04ba67592408

Source dataset

uspto-grants-1991_04

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US05008267