Sodium Hydroxide → 1,2,3-Trichlorobenzene

Temperature

170 °C

Chlorine gas (400 mg, 573 millimoles) was bubbled into a solution of benzenephosphorusdichloride (789 microliters, 573 millimoles) in BPOD (10 ml) at room temperature. The initially clear colorless solution became warm and turned pale yellow, but remained clear. To this mixture was added 1,2-dichloro-3-nitrobenzene (1.0 g, 573 millimoles) and then the reaction mixture was heated to 170° C. for 5 hours. The cooled reaction mixture was then poured onto crushed ice/water (100 ml) and neutralized with 50% aqueous sodium hydroxide. After extracting with ether, the ether extracts were dried and concentrated in vacuo to yield 1,2,3-trichlorobenzene (880 mg, 94 weight %).

1. temperatureThe initially clear colorless solution became warm
2. customThe cooled reaction mixture
3. additionwas then poured
4. extractionAfter extracting with ether
5. dry with materialthe ether extracts were dried
6. concentrationconcentrated in vacuo

ORD record

ord-3aa30f4fba9e4053b59cc80d7fbe36b8

Source dataset

uspto-grants-1988_03

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US04730046