Isopropanol → HCID 23447873, compound

Temperature

60 °C

A mixture of 1.0 g of 4-chloro-2-fluoronitrobenzene and 9.3 g of caesium carbonate in 10 ml of 2-propanol is heated at 60° C. for 24 h. The mixture is then concentrated and the residue is taken up with 100 ml of a mixture of water and ethyl acetate. The aqueous phase is extracted three times with 50 ml of ethyl acetate. The combined organic phases are washed with 50 ml of a saturated sodium chloride solution, dried over anhydrous magnesium sulfate, filtered and then concentrated to dryness under reduced pressure. The residue is purified on 90 g of silica, elution being carried out with 95/5 heptane/ethyl acetate, so as to obtain 885 mg of 4-chloro-1-nitro-2-(propan-2-yloxy)benzene in the form of a yellow solid.

1. concentrationThe mixture is then concentrated
2. extractionThe aqueous phase is extracted three times with 50 ml of ethyl acetate
3. washThe combined organic phases are washed with 50 ml of a saturated sodium chloride solution
4. dry with materialdried over anhydrous magnesium sulfate
5. filtrationfiltered
6. concentrationconcentrated to dryness under reduced pressure
7. customThe residue is purified on 90 g of silica, elution

ORD record

ord-90b48f35d0934e5cb9ef2196a7c83761

Source dataset

uspto-grants-2015_08

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US09115140B2