Nitric Acid → 2,5-Bis(2,2,2-trifluoroethoxy)nitrobenzene

To 58.1 g. (0.212 mole) of 1,4-bis(2,2,2-trifluoroethoxy)benzene in 400 ml. of trifluoroacetic acid is added dropwise with stirring 13.7 ml. of concentrated nitric acid over 3.5 hours at 25± 2° C. Stirring is continued for 24 hours, then the mixture is concentrated to one-third the original volume. The concentrate is poured into 600 ml. of water, and the resulting solution is extracted twice with diethyl ether. The ether solution is washed thrice with saturated sodium chloride solution, then with dilute sodium hydroxide solution until the washings are basic. The solution is washed again with saturated sodium chloride solution, dried and evaporated. The liquid residue is distilled to provide 2,5-bis(2,2,2-trifluoroethoxy)nitrobenzene as a clear, pale yellow liquid, b.p. 116°-119° C/0.35 mm Hg.

1. stirringStirring
2. concentrationthe mixture is concentrated to one-third the original volume
3. additionThe concentrate is poured into 600 ml
4. extractionof water, and the resulting solution is extracted twice with diethyl ether
5. washThe ether solution is washed thrice with saturated sodium chloride solution
6. washThe solution is washed again with saturated sodium chloride solution
7. customdried
8. customevaporated
9. distillationThe liquid residue is distilled

ORD 기록

ord-80bd73cb3232416b83ceef08b4b7b0d6

출처 데이터셋

uspto-grants-1979_05

DOI

10.6084/m9.figshare.5104873.v1

특허 번호

US04154941