Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
HRID 1168412생성일: 2026년 10월 26일
Sodium Carbonate → alpha-(4-tert-Butylphenyl)-beta-[(methylthio)carbonyloxy]-beta-(2-trifluoromethylphenyl)acrylonitrile
https://huagongshe.com/reaction/1168412
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Sodium Carbonate | HCID 10340 | — |
| 반응물 | Methyl 3-chlorothiophene-2-carboxylate | HCID 2777566 | — |
| 반응물 | alpha-(4-Tert-butylphenyl)-beta-hydroxy-beta-(2-trifluoromethylphenyl)acrylonitrile | HCID 70026415 | — |
| 용매 | Acetone | HCID 180 | — |
| 생성물 | alpha-(4-tert-Butylphenyl)-beta-[(methylthio)carbonyloxy]-beta-(2-trifluoromethylphenyl)acrylonitrile | HCID 86759172 | 96.2% |
반응 단계
A mixture comprising 5.0 g of α-(4-tert-butylphenyl)-β-hydroxy-β-(2-trifluoromethylphenyl)acrylonitrile, 2.0 g of sodium carbonate and 30 ml of acetone, was heated, and a mixture comprising 2.1 g of methyl chlorothiolformate and 10 ml of acetone, was dropwise added over a period of 10 minutes under reflux. After completion of the dropwise addition, the reaction was carried out for 60 minutes under reflux. The reaction mixture was cooled, and then, an inorganic salt was filtered off. The cake was washed with 20 ml of acetone. Acetone in the filtrate was distilled off, and 50 ml of ISOPAR G (tradename) was added to the residue, followed by heating and dissolution. Then, the solution was left to cool to room temperature. Precipitated crystals were collected by filtration, and the cake was washed with 10 ml of ISOPAR G (tradename) and then dried at 45° C. for 12 hours to obtain 4.8 g of the desired product (isomer ratio 0:100). The HPLC conditions for the analysis of this product were the same as in Preparation Example 5. Further, the NMR spectrum data of this product were the same as the geometrical isomer having a longer retention time of Preparation Example 4.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US06624179B1 |
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| 출처 데이터셋 | uspto-grants-2003_09 |
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| ORD ID | ord-a0c183d16c06471480f605368111bbd1 |
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| 출처 메모 | uspto-grants-2003_09 |
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