Benzene → Benzene, 1-isocyano-4-nitro-

p-nitroaniline (5 gms; 0.036 mole) and potassium-t-butoxide (20 gms; 0.18 mole) were dissolved with stirring in t-butanol (1 liter). Chloroform (8 ml: 0.07 mole) was then added dropwise and the reaction allowed to proceed with stirring for 1 hr. Benzene (200 ml) and water were added until phase separation occured. The benzene phase was separated. The aqueous phase was extracted with two 100 ml portions of benzene. The combined benzene extract was washed with water and concentrated to a final volume of about 100 ml. in a rotatory evaporator. The concentrated benzene solution was passed through an activated-alumina column (2.5 × 25 cm), the yellow-orange fractions collected and evaporated to dryness. The yellowish brown solid (3.5 gms; 60% yield) was stored in a closed vessel, at -5°.

1. customThe benzene phase was separated
2. extractionThe aqueous phase was extracted with two 100 ml portions of benzene
3. extractionThe combined benzene extract
4. washwas washed with water
5. concentrationconcentrated to a final volume of about 100 ml
6. customin a rotatory evaporator
7. customthe yellow-orange fractions collected
8. customevaporated to dryness
9. customThe yellowish brown solid (3.5 gms; 60% yield) was stored in a closed vessel, at -5°

ORD record

ord-3c29f84a33a142c88d811e9ca0d6a965

Source dataset

uspto-grants-1976_07

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US03970597