Hexane → HCID 22388299, compound

2,3,4-Trichlorotoluene (2.00 g) was dissolved in carbon tetrachloride (20 ml), and 2,2′-azobis(2,4-dimethyl-4-methoxyvaleronitrile) (158 mg) and N-bromosuccinimide (2.00 g) were added thereto. The mixture was refluxed under heating for 2 hr, and hexane was added, which was followed by stirring under cooling for 30 min. The mixture was filtrated and an insoluble matter on a filter paper was washed with small amounts of hexane. The filtrates were combined and concentrated under reduced pressure. Diisopropyl ether was added to the residue and the mixture was washed successively with a saturated aqueous sodium hydrogencarbonate solution and saturated brine, dried over anhydrous magnesium sulfate and filtrated. The filtrate was concentrated under reduced pressure to give a mixture (2.40 g) of the objective compound and 2,3,4-trichlorotoluene as brown crystals.

1. temperatureThe mixture was refluxed
2. temperatureunder heating for 2 hr
3. temperatureunder cooling for 30 min
4. filtrationThe mixture was filtrated
5. washan insoluble matter on a filter paper was washed with small amounts of hexane
6. concentrationconcentrated under reduced pressure
7. additionDiisopropyl ether was added to the residue
8. washthe mixture was washed successively with a saturated aqueous sodium hydrogencarbonate solution and saturated brine
9. dry with materialdried over anhydrous magnesium sulfate
10. filtrationfiltrated
11. concentrationThe filtrate was concentrated under reduced pressure

ORD record

ord-244e3c053e5d40fb874b416bc516eeab

Source dataset

uspto-grants-2002_02

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US06348474B1