Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Methacryloyl chloride | HCID 13528 | — |
| Reactant | 2,6-Di-tert-butyl-4-methylphenol | HCID 31404 | — |
| Reactant | HCID 67586083 | HCID 67586083 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 67586751 | HCID 67586751 | — |
Reaction Steps
2-acetyl-4-hydroxysalicylic acid (15.0 millimole, 2.9 g) and butylhydroxytoluene (10 mg) was dissolved in tetrahydrofuran (THF). To the solution was added triethylamine (0.5 g), and the solution was cooled to 0° C. by ice bath. While stirring under a flow of nitrogen gas, methacryl chloride (20 millimole, 2.41 g) was added to the solution using a syringe over a period of 20 minutes, and the solution was kept stirred for another hour after completing the addition. After the reaction was over, the solvent was evaporated to give pale yellow powder. The powder was washed by dichloromethane and recrystallized by an aqueous solution of 0.5% hydroquinone. Dried under a reduced pressure, colorless crystal having a needle shape was obtained: m.p. 152.7° C.; yield 2.54 g, 64.1%.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US05693320 |
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| Source dataset | uspto-grants-1997_12 |
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| ORD ID | ord-d7f206f9c3b44f2380d6805538f76f78 |
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| Source note | uspto-grants-1997_12 |
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