SILICON(IV) PHTHALOCYANINE BIS(TRIHEXYL& synthesis
- Product Name:SILICON(IV) PHTHALOCYANINE BIS(TRIHEXYL&
- CAS Number:92396-89-9
- Molecular formula:C68H94N8O2Si3
- Molecular Weight:1139.81
Yield:92396-89-9 93%
Reaction Conditions:
with sodium hydroxide;Aliquat HTA-1 in chlorobenzene at 132; for 6 h;Product distribution / selectivity;
Steps:
3.a
a) 2.87 g (4.7 mmol) of silicon phthalocyanine dichloride, 4.93 g (15.0 mmol) of chlorotri-n-hexylsilane, 1.00 g (25.0 mmol) of sodium hydroxide (powder) and 0.04 g of Aliquat HTA-1 (Cognis) were heated to boiling (132° C.) under reflux in 25 ml of chlorobenzene. After one hour, another 1.64 g (5.0 mmol) of chlorotri-n-hexylsilane were added and, after a further hour, another 1.64 g (5.0 mmol) of chlorotri-n-hexylsilane and 0.40 g (10 mmol) of sodium hydroxide (powder). After heating at reflux temperature for a further 4 hours, the solution was allowed to cool to room temperature. The solution was filtered, which left a residue. The filtrate was concentrated to dryness and then admixed with methanol. The solid was filtered off with suction, washed with methanol and water and dried at 50° C. under reduced pressure. 5.05 g of blue powder were obtained, which comprised 99 mol % of material of value (UV/Vis). The calculated material of value yield was 93% of theory.UV/Vis (toluene): λmax=668 nm, mass extinction ME=335.1 l/(g*cm), λem=671 nm.
References:
US2010/113767,2010,A1 Location in patent:Page/Page column 11
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