참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | 2-Pyridinemethanamine | HCID 19509 | — |
| 반응물 | 2,5-bis(2,2,2-trifluoroethoxy)benzoic Acid | HCID 2736078 | — |
| 용매 | Ethyl Acetate | HCID 8857 | — |
| 생성물 | 2,5-Bis(2,2,2-trifluoroethoxy)-N-(2-pyridylmethyl)benzamide | HCID 93669 | 685.8% |
반응 단계
To a solution of 8.93 g (2.5 mmole) of compound (II) in 80 mL of ethyl acetate under argon, 2-(aminomethyl)pyridine (3.2 g, 3.0 mmole) were added with stirring and the mixture was refluxed for 4 hours. An additional 1 g of 2-(aminomethyl)pyridine was added and the mixture was refluxed for two more hours. The ethyl acetate was evaporated under reduced pressure and the residue was passed through a 12 cm column containing silica gel with a mixture of methylene chloride:hexane (1:1) as eluent. The column was washed with methylene chloride and the combined solutions were evaporated under reduced pressure. The residue was crystallized from CH2CI2:hexane (1:2) to give 7 g (69% yield) of 2,5-bix(2,2,2-trifluoroethoxy)-N-(2-pyridylmethyl)benzamide (V) m.p. 104-106° C., purity 99.8% (GC).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US06538138B1 |
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| 출처 데이터셋 | uspto-grants-2003_03 |
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| ORD ID | ord-9e7ba310ce8e458888cbf5ec50eeba43 |
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| 출처 메모 | uspto-grants-2003_03 |
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