Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydroquinone | HCID 785 | — |
| Reactant | Glycidyl methacrylate | HCID 7837 | — |
| Catalyst | Heptanoic acid, chromium(3+) salt (3:1) | HCID 173191 | — |
| Solvent | O-Xylene | HCID 7237 | — |
| Product | HCID 131734266 | HCID 131734266 | — |
Reaction Steps
A mixture of 9.95 g of glycidyl methacrylate, 4.40 g of hydroquinone, 0.050 g of HEPTCR 050 NPG (chromium heptanoate in polypropylene glycol) and 50 ml of o-xylene is initially charged in a 250 ml four-neck flask with a sabre stirrer (stirrer sleeve, stirrer motor), a thermometer, an inlet tube for compressed air, a reflux condenser and an oil bath with temperature regulation. The reaction mixture was heated to boiling with introduction of air. This was followed by refluxing at a reaction temperature (=internal flask temperature) of 142° C. for 10 h. After cooling to room temperature, the volatile constituents were removed in a rotary evaporator (bath temperature 55° C., vacuum 20 mbara). After filtration, a brown, cloudy liquid was obtained. The synthesis product was purified by means of column and thin-layer chromatography. The stationary phase used for column chromatography was silica gel 60 (0.063-0.200 mm); the eluent consisted of an ethyl acetate/cyclohexane mixture in a ratio of 1/1. The clear and colourless solutions obtained were combined to give three fractions. The eluent was subsequently removed on a rotary evaporator.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US09206112B2 |
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| Source dataset | uspto-grants-2015_12 |
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| ORD ID | ord-2386a8dfde05492fa3007e85f0673d24 |
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| Source note | uspto-grants-2015_12 |
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