関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Acetic Acid | HCID 176 | — |
| 反応物 | Dimethyl Sulfoxide | HCID 679 | — |
| 反応物 | (E)-1-(Benzyloxy)-4-(2-nitrovinyl)benzene | HCID 5702926 | — |
| 反応物 | Vertellus | HCID 22959485 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 1-Benzyloxy-4-(2-nitro-ethyl)-benzene | HCID 24721037 | — |
反応手順
While cooling using a water bath, to a mixture of 1-benzyloxy-4-((E)-2-nitro-vinyl)-benzene described in Manufacturing Example 229-1-1 (60 g, 0.23 mol), acetic acid (27 mL) and dimethyl sulfoxide (400 mL) was added sodium borohydrate (8.9 g, 0.23 mol), which was stirred for 20 minutes at room temperature. Water (2.5 L) was added dropwise to the reaction mixture, and the deposited solids were filtered. Diethyl ether (300 mL) was added to the obtained solids to dissolve the title compound, and separation into filtrate and solids was carried out by filtration. The filtrate was concentrated under a reduced pressure to obtain the title compound (39 g). On the other hand, diethyl ether (300 mL) was added to the previously separated solid to dissolve the title compound, and separation into filtrate and solids was carried out by filtration. The filtrate was concentrated under a reduced pressure to obtain the title compound (12 g). This was combined with the previously obtained solids to obtain the title compound (51 g) as a crude product.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 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-a3349ff6394d4fd3981d78e8162ad706 |
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| 出典メモ | uspto-grants-2014_09 |
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