Nitric Acid → 1-(2,2-Dichlorocyclopropyl)-4-nitrobenzene

Temperatur

4 °C

Nitric acid (25 g.) was added during three hours to a mixture of (2,2-dichlorocyclopropyl)benzene (45 g.), water (13 g.), acetic acid (40 g.) and concentrated sulfuric acid (177 g.) with cooling (to 3-5° C.). The resulting mixture was quenched in a mixture of ice (400 g.) and chloroform (200 g.). The layers were separated and the aqueous layer was washed with chloroform (100 g.). The chloroform layers were combined and washed with aqueous sodium carbonate (5%, 300 ml.). The sodium carbonate layer was backwashed with chloroform (75 g.). The combined chloroform extracts were dried, fitered and concentrated, affording p-(2,2-dichlorocyclopropyl)nitrobenzene mixed with the ortho isomer (57 g.).

1. customThe resulting mixture was quenched in a mixture of ice (400 g.) and chloroform (200 g.)
2. customThe layers were separated
3. washthe aqueous layer was washed with chloroform (100 g.)
4. washwashed with aqueous sodium carbonate (5%, 300 ml.)
5. dry with materialThe combined chloroform extracts were dried
6. concentrationconcentrated

ORD-Eintrag

ord-250df96471cb4983aa8c537adc700a64

Quelldatensatz

uspto-grants-1977_10

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US04053636