2-(3-OXO-1,3-DIHYDROISOBENZOFURAN-1-YLIDEN)ACETIC ACID synthesis
- Product Name:2-(3-OXO-1,3-DIHYDROISOBENZOFURAN-1-YLIDEN)ACETIC ACID
- CAS Number:4743-57-1
- Molecular formula:C10H6O4
- Molecular Weight:190.15
Yield:4743-57-1 48%
Reaction Conditions:
with potassium acetate at 140 - 150; for 0.5 h;
Steps:
pp28.2.p1
Phthalic anhydride (751.5 g, 5.014 mole), potassium acetate (498 g, 5.014 mole) and acetic anhydride (1 L) were stirred together under nitrogen. The mixture was slowly warmed to 145-150° C. and stirred for 10 minutes, then at 140° C. for 20 minutes. The mixture was allowed to slowly cool to 80° C. over 1 hour. Three volumes of water were added causing precipitation of a solid. After filtration, the filtered solid was washed with warm water and pulled as dry as possible for 30 minutes. The solid was then washed with ethanol and acetone respectively. If required further purification could be achieved by slurring the solid in acetone, at room temperature, for 15 minutes, then filtration. Drying in vacuo at 50° C. for 20 hours gave compound 2 as an off-white solid, 470 g (48%) with an NMR purity of approx. 90%.
References:
US2004/82590,2004,A1 Location in patent:Page/Page column 97
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