참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Nitromethane | HCID 6375 | — |
| 반응물 | Ammonium Acetate | HCID 517165 | — |
| 반응물 | 4-(6-Methyl-pyridin-2-yloxymethyl)-benzaldehyde | HCID 59255148 | — |
| 용매 | Acetic Acid | HCID 176 | — |
| 생성물 | 2-Methyl-6-(4-((E)-2-nitro-vinyl)-benzyloxy)-pyridine | HCID 59255368 | 110% |
반응 단계
To a solution of 4-(6-methyl-pyridin-2-yloxymethyl)-benzaldehyde (4.19 g, 18.5 mmol) described in Manufacturing Example 3-1-2 in acetic acid (30 mL) were added nitromethane (5.65 g, 92.6 mmol) and ammonium acetate (2.85 g, 37.0 mmol) under nitrogen atmosphere, which was stirred for 3 hours at 110° C. The reaction mixture was partitioned into water and ethyl acetate. The organic layer was washed with water and saturated aqueous sodium chloride, and dried over anhydrous magnesium sulfate, and the solvent was evaporated under a reduced pressure to obtain the title compound (5.50 g) as a crude product.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08841327B2 |
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| 출처 데이터셋 | uspto-grants-2014_09 |
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| ORD ID | ord-8d3d40763f0c4de1a07f9332ef3d77f1 |
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| 출처 메모 | uspto-grants-2014_09 |
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