참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Acetoin | HCID 179 | — |
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | Methacryloyl chloride | HCID 13528 | — |
| 촉매 | 4-Methoxyphenol | HCID 9015 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | HCID 19357483 | HCID 19357483 | 53.1% |
반응 단계
In a 2 L four-necked flask subjected replacement with nitrogen, 150 g of 3-hydroxy-2-butanone (made by Tokyo Chemical Industry Co., Ltd., purity: 95.0% or more) was put, and dissolved in 750 g of methylene chloride, and a stirrer, a thermometer and a Dimroth cooling tube were connected thereto. After the solution was stirred and cooled to about 5° C., 190 g of triethylamine and 80 mg of p-methoxyphenol were added thereto. While the solution was cooled to about 5° C. under stirring, 178 g of methacryloyl chloride was slowly added dropwise thereto over 4 hours, and further stirred for 30 minutes after completion of the dropwise addition to allow a reaction. The resulting reaction mixture was washed with 1 N-hydrochloric acid, a 10% sodium carbonate aqueous solution and saturated brine at room temperature, dried over anhydrous magnesium sulfate and separated by filtration to obtain a reaction crude liquid. The solvent of the reaction crude liquid was distilled off using an evaporator, 80 mg of p-methoxyphenol was added thereto and the resulting solution was distilled under reduced pressure to give 141 g of 3-oxobutane-2-yl methacrylate of 96.5% GC purity (yield: 53.1% based on 3-hydroxy-2-butanone).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US09346775B2 |
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| 출처 데이터셋 | uspto-grants-2016_05 |
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| ORD ID | ord-33fe739cceb54b13a9279ebb70c7a281 |
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| 출처 메모 | uspto-grants-2016_05 |
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