참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Nitromethane | HCID 6375 | — |
| 반응물 | Ammonium Acetate | HCID 517165 | — |
| 반응물 | 4-(Pyridin-2-ylmethoxy)benzaldehyde | HCID 759667 | — |
| 용매 | Acetic Acid | HCID 176 | — |
| 생성물 | 2-(4-((E)-Nitro-vinyl)-phenoxymethyl)-pyridine | HCID 59255195 | 97.3% |
반응 단계
A mixture of 4-(pyridin-2-ylmethoxy)-benzaldehyde (29 g, 136 mmol) described in Manufacturing Example 203-1-1, nitromethane (36.6 mL, 680 mmol), ammonium acetate (21 g, 272 mmol), and acetic acid (300 mL) was stirred for 21 hours at 100° C. This mixture was cooled to room temperature and concentrated under a reduced pressure. The residue was partitioned into ethyl acetate and water. The organic layer was separated, washed with water and saturated aqueous sodium chloride, dried over anhydrous magnesium sulfate, and filtered. The filtrate was concentrated under a reduced pressure to obtain the title compound (33.9 g, 97%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07691882B2 |
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| 출처 데이터셋 | uspto-grants-2010_04 |
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| ORD ID | ord-908afebde5b3447283528a5f13508498 |
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| 출처 메모 | uspto-grants-2010_04 |
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