참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Pyridine | HCID 1049 | — |
| 반응물 | Ethyl 3-(N,N-dimethylamino)acrylate | HCID 121015 | — |
| 반응물 | HCID 10610913 | HCID 10610913 | — |
| 촉매 | Ethyl Acetate | HCID 8857 | — |
| 용매 | Ethyl Acetate | HCID 8857 | — |
| 생성물 | Ethyl 2-(2,4,5-trifluoro-3-methyl-6-nitrobenzoyl)-3-dimethylaminoacrylate | HCID 72820967 | 100.5% |
반응 단계
1.4 g (0.01 mol) of ethyl 3-dimethylaminoacrylate, 15 mg of ethyl acetate and 0.8 mg (0.01 mol) of pyridine were loaded and cooled below 5° C., and a liquid mixture of 3 g (0.01 mol) of 2,4,5-trifluoro-3-methyl-6-nitrobenzoyl chloride and 5 ml of ethyl acetate was added dropwise while the temperature was maintained at 0 to 5° C. The resulting mixture was stirred at 5° C. for 1 hour and then stirred at room temperature (25° C.) overnight (12 hours). The precipitated pyridine hydrochloride was filtered off, and the filtrate was concentrated under reduced pressure to give 3.62 g of ethyl 3-dimethylamino-2-(2,4,5-trifluoro-3-methyl-6-nitrobenzoyl)acrylate with a 87% purity (in terms of the percentage of the peak area in HPLC) as the residue.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US06531624B1 |
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| 출처 데이터셋 | uspto-grants-2003_03 |
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| ORD ID | ord-d6e6b984bd674c68a064086fea3d5f04 |
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| 출처 메모 | uspto-grants-2003_03 |
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