Hexachloroethane → Benzene, 1-methyl-3-(trichloromethyl)-

Temperatur

90 °C

36.2 gms of 3-methyl benzal chloride in 207 gms of solvent, tetrachloroethylene, was added into a reaction vessel with 53.9 gms of hexachloroethane, 66.3 gms of 50% sodium hydroxide, and 1.4 gms of Aliquot 4. The mixture was stirred and refluxed under partial vacuum at about 90° C. for about 1 hour. 20.3 ml of water was removed from the mixture via a Dean Stark trap during this period. The mixture was refluxed for another hour an additional 10.5 ml of water was removed. 200 ml of water was added to the cooled mixture and 15 gms of HCl gas was added until the mixture turned acidic. After standing for 2 days, the organic layer was removed and the tetrachloroethylene was distilled off under reduced pressure. The remaining residue was then distilled to give 36.7 gms of a clear oil. b.p. 80° -90° C. (0.6-1.0 mm/Hg-0.8-1.33×105 pascals). (Yield 85% - 97.2 assay).

1. custom20.3 ml of water was removed from the mixture via a Dean Stark trap during this period
2. temperatureThe mixture was refluxed for another hour an additional 10.5 ml of water
3. customwas removed
4. addition200 ml of water was added to the cooled mixture and 15 gms of HCl gas
5. additionwas added until the mixture
6. customthe organic layer was removed
7. distillationthe tetrachloroethylene was distilled off under reduced pressure
8. distillationThe remaining residue was then distilled

ORD-Eintrag

ord-6637a25f11cc4419aa073630bb794b8f

Quelldatensatz

uspto-grants-1986_06

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US04593144