참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | Bromoxynil | HCID 15531 | — |
| 반응물 | 2-Fluoroacryloyl chloride | HCID 2783335 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | 2,6-Dibromo-4-cyanophenyl alpha-fluoroacrylate | HCID 14008161 | 55.7% |
반응 단계
10 g (0.092 mol) α-fluoroacryloyl chloride (obtained in accordance with example 1c) were added dropwise, at a temperature of 5° C., with stirring and in the course of 5 minutes, to a solution of 24.8 g (0.09 mol) of 3,5-dibromo-4-hydroxybenzonitrile and 9.1 g (0.09 mol) of triethylamine in 200 ml of anhydrous methylene dichloride, and the reaction mixture was then stirred for a further 30 minutes at the same temperature. The solid formed was filtered off and washed with 20 ml of anhydrous methylene dichloride. After 0.005 g of hydroquinone monomethyl ether had been added, the volatile constituents in the mixture of filtrate and wash solution were removed by distillation, and the residue was recrystallized from boiling n-heptane. 17.5 g (55% of theory) of 2,6-dibromo-4-cyanophenyl α-fluoroacrylate were obtained, melting point 135° to 138° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US05266668 |
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| 출처 데이터셋 | uspto-grants-1993_11 |
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| ORD ID | ord-ad66178dc3904c1b86ff0330f8ddf9e2 |
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| 출처 메모 | uspto-grants-1993_11 |
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