Toluene → HCID 87097284, compound
Reaction equation
[Ti:1]([Cl:5])([Cl:4])([Cl:3])[Cl:2].[C:6]1([CH3:12])[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1>>[Ti:1]([Cl:5])([Cl:4])([Cl:3])[Cl:2].[C:6]1([CH3:12])[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1Participants
Procedure
To the above described solid component were added 40 ml of toluene and titanium tetrachloride was then added thereto to give a titanium tetrachloride/toluene volume ratio of 3/2, followed by raising the temperature to 90° C. Under stirring, a mixed solution of 2 ml of di-n-butyl phthalate and 5 ml of toluene was dropwise added thereto for 5 minutes and stirred for 2 hours at 120° C. The thus resulting solid material was separated by filtration at 90° C. and washed 2 times with 100 ml of toluene at 90° C. Further, titanium tetrachloride was newly added to give a titanium tetrachloride/toluene volume ratio of 3/2 and stirred at 120° C. for 2 hours. The resulting solid material was separated by filtration at 110° C. and washed 7 times respectively with 100 ml of n-hexane at room temperature to obtain 5.5 g of Component A.
Workup
- additionwas then added
Sources & evidence
- ORD record
- ord-9f80ed2118544e17a5ab4e3df853daad
- Source dataset
- uspto-grants-1993_01
- Patent number
- US05177043
Reaction notes
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