Durene → Titanium Dichloride Aluminum Chloride Durene

Temperature

130 °C

20 g of aluminum power (BDH fine powder) and 27 g of aluminum chloride were introduced into a two liter flask. The mixture of solids was stirred and heated to a temperature of 130° C., which temperature was maintained for two hours. The mixture was then cooled, and a solution of 15.5 g of durene in one liter of toluene was added. The flask contents were stirred and heated to reflux temperature. 19.9 g of titanium tetrachloride in 100 ml of toluene were added dropwise over a period of 30 minutes. Heating was continued, at reflux temperature, for a further hour and the mixture was then allowed to cool. The mixture was then filtered and the filtrate was allowed to run directly into 2.5 liters of n-heptane. A dark-colored precipitate separated out and was filtered and then washed four times with 250 ml of n-heptane for each wash. The precipitate was then dried under vacuum (0.2 mm pressure) at ambient temperature (about 20° C.).

1. additionThe mixture of solids
2. temperaturewas maintained for two hours
3. temperatureThe mixture was then cooled
4. stirringThe flask contents were stirred
5. temperatureheated
6. temperatureto reflux temperature
7. temperatureHeating
8. temperatureat reflux temperature
9. waitfor a further hour
10. temperatureto cool
11. filtrationThe mixture was then filtered
12. customA dark-colored precipitate separated out and
13. filtrationwas filtered
14. washwashed four times with 250 ml of n-heptane for each wash
15. customThe precipitate was then dried under vacuum (0.2 mm pressure) at ambient temperature (about 20° C.)

ORD record

ord-e87b029bcf9049b08e1616b05e29b129

Source dataset

uspto-grants-1981_11

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US04299936