Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Methacrylic Acid | HCID 4093 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | 2,6-Di-tert-butyl-4-methylphenol | HCID 31404 | — |
| Reactant | HCID 9943182 | HCID 9943182 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | HCID 12040555 | HCID 12040555 | — |
Reaction Steps
A flask equipped with a stirrer, reflux condenser, dropping funnel and thermometer was charged with 17.2 g (0.2 mol) of methacrylic acid, 120 ml of toluene, and 0.06 g of 2,6-di-tert-butyl-4-methylphenol. At room temperature, 22.3 g (0.22 mol) of triethylamine was added dropwise over one hour. At the end of dropwise addition, the flask was heated at 80° C. After the internal temperature became constant, 52.6 g (0.20 mol) of thexyldiisobutylchlorosilane was added dropwise over two hours. After the completion of dropwise addition, the reaction solution was stirred for 5 hours at 80° C. The reaction solution was then cooled to room temperature, and the resulting hydrochloric acid salt removed by filtration. The filtrate was distilled, collecting 46.3 g of a fraction having a boiling point of 104-110° C./0.13 kPa.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06498264B2 |
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| Source dataset | uspto-grants-2002_12 |
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| ORD ID | ord-19f5ef2576dc4c4c8d65d90a0c9d47b3 |
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| Source note | uspto-grants-2002_12 |
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