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Acenaphthene-5,6-dicarboxylic anhydride synthesis
- Product Name:Acenaphthene-5,6-dicarboxylic anhydride
- CAS Number:5699-00-3
- Molecular formula:C14H8O3
- Molecular Weight:224.21
![5,6-Acenaphthylenedicarboxamide,1,2-dihydro-N5,N5,N6,N6-tetramethyl-](/CAS/20180601/GIF/31458-06-7.gif)
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Yield:5699-00-3 68.7%
Reaction Conditions:
with hydrogenchloride;lithium hydroxide monohydrateReflux;
Steps:
1A Synthesis of 1,2-dihydroacenaphthylene dicarboxylic acid anhydride.
Synthesis of 1,2-dihydroacenaphthylene dicarboxylic acid anhydride. N5 ,N5 ,N6,N6-tetramethyl- 1 ,2-dihydroacenaphthylene-5 ,6-dicarboxamide (4.0 g, 13.5 mmol) was suspended in 10 mL of concentric hydrochloric acid. The mixture was heated to reflux for 4-5 hours. The solution was then cooled to 0 °C. The off-white precipitate was collected by filtration and washed with cold water. The crude materials were recrystallized from hot acetic anhydride solution to afford pure product as light brown needles. Yield (2.08 g, 68.7%). ‘H NMR (CDC13, 500.046 MHz): 8= 8.54 (d, 2H, 3J = 7.0 Hz, Np), 7.65 (d, 2H, 3J =7.0 Hz, Np), 3.45 (s, 4H, CH2).
References:
WO2014/31750,2014,A1 Location in patent:Page/Page column 40
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