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ChemicalBook CAS DataBase List TITANIUM(IV) PHTHALOCYANINE DICHLORIDE
16903-42-7

TITANIUM(IV) PHTHALOCYANINE DICHLORIDE synthesis

3synthesis methods
-

Yield:-

Reaction Conditions:

with 1,8-diazabicyclo[5.4.0]undec-7-ene in pentan-1-ol; for 7 h;Heating / reflux;

Steps:

2 Synthesis Example 2; Synthesis of titanyl phthalocyanine O=TiPc

Synthesis Example 2 Synthesis of titanyl phthalocyanine O=TiPc (A method described in Example 1 of Japanese Patent Laid-Open Publication No. H3(1991) 21669) 91.8 g (approximately 0.6 mol) of 1,8-diazabicyclo[5,4,0]unde-7-cene (DBU) was dropped into a mixture of 76.2 g (approximately 0.6 mol) of phthalonitrile, 56.4 g (approximately 0.3 mol) of titanium tetrachloride and 200 ml of n-amyl alcohol under heat-reflux for approximately 1 hour, and further stirred under heat-reflux for 6 hours. After the reaction was completed, the mixture stood to cool to a temperature of 100C, approximately 30 ml of water was added thereto, and it was stirred for a while, and thereafter the product was filtered, sprinkled and washed with 100 ml of dimethylformamide (DMF) and subsequently 100 ml of methanol. The obtained dichlorotitanium phthalocyanine was dispersed into 1000 ml of 3%-hydrochloric acid and washed with water so that pH becomes 6 or more. Next, this water-wet cake was put into approximately 500 ml of DMF previously heated to a temperature of 100 to 120C, stirred at this temperature for approximately 1 hour, and thereafter filtered under heating. The obtained DMF-wet cake was washed with 100 ml of methanol, dried to obtain 29.1 g of titanyl phthalocyanine O=TiPc.

References:

EP1418207,2004,A1 Location in patent:Page 8

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