Benzene → HCID 86736249, compound

Temperature

130 °C

51 grams of aluminum powder (BDH fine powder) and 80 grams of anhydrous aluminum chloride were introduced into a 2 liter, three-necked flask and the mixture of solids was heated at 130° C. for 0.5 hours. The mixture was then allowed to cool. 500 ml of benzene was added and then 33.3 grams of titanium tetrachloride was added with stirring. The mixture was refluxed for 20 hours and then allowed to cool. The cool solution was filtered into 1 liter of heptane, and this mixture was cooled to -10° C. and maintained at this temperature for 24 hours. The supernatant liquid was decanted from the purple solid which had been formed. The solid was washed four times using 1 liter of heptane for each wash, and then was dried under reduced pressure (1 mm mercury) at ambient temperature.

1. additionthe mixture of solids
2. temperatureto cool
3. temperatureThe mixture was refluxed for 20 hours
4. temperatureto cool
5. filtrationThe cool solution was filtered into 1 liter of heptane
6. temperaturethis mixture was cooled to -10° C.
7. temperaturemaintained at this temperature for 24 hours
8. customThe supernatant liquid was decanted from the purple solid which
9. customhad been formed
10. washThe solid was washed four times
11. dry with materialwas dried under reduced pressure (1 mm mercury) at ambient temperature

ORD record

ord-c82ed0a6c4a8421ba1b39cec3e747b1d

Source dataset

uspto-grants-1979_01

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US04136057