関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Acetic Acid | HCID 176 | — |
| 反応物 | Nitromethane | HCID 6375 | — |
| 反応物 | Ammonium Acetate | HCID 517165 | — |
| 反応物 | 4-(5-Methyl-pyridin-2-yloxymethyl)-benzaldehyde | HCID 59255142 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | HCID 59255428 | HCID 59255428 | 100.4% |
反応手順
To an acetic acid (20.0 mL) solution of 4-(5-methyl-pyridin-2-yloxymethyl)-benzaldehyde (2.93 g, 12.9 mmol) described in Manufacturing Example 44-1-2 were added nitromethane (3.94 g, 64.5 mmol) and ammonium acetate (1.99 g, 25.8 mmol) under nitrogen atmosphere at room temperature, which was stirred for 2.5 hours at 100° C. Water and ethyl acetate were added to the reaction mixture, and the organic layer was extracted with ethyl acetate. This organic layer was 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 (3.50 g) as a crude product.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08841327B2 |
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| 出典データセット | uspto-grants-2014_09 |
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| ORD ID | ord-e6256274e4a94f8cafdaaaa5fc21d1c1 |
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| 出典メモ | uspto-grants-2014_09 |
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