関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | 2-Chloro-5-(chloromethyl)pyridine | HCID 155479 | — |
| 反応物 | 4-(methylamino)furan-2(5H)-one | HCID 12213511 | — |
| 溶媒 | 1,2-Dimethoxyethane | HCID 8071 | — |
| 生成物 | 4-[[(6-chloropyridin-3-yl)methyl](methyl)amino]furan-2(5H)-one | HCID 11550459 | 87% |
反応手順
30 g of 4-(methylamino)furan-2(5H)-one (Example 11) are initially charged in 450 ml of dimethoxyethane at room temperature. Subsequently, 12.6 g of sodium hydroxide are added and, at 40° C., 225 g of a 20% solution of 2-chloro-5-(chloromethyl)pyridine in dimethoxyethane are metered in. The mixture is stirred at 50° C. for a further 6 h. The solvent is substantially removed under reduced pressure and the residue is admixed with 300 ml of water. The solids are filtered off, washed with 150 ml of water and dried under reduced pressure. 58.7 g of 4-([[6-chloropyridin-3-yl]methyl](methy)amino)furan-2(5H)-one are obtained with a purity of 94% (this corresponds to 87% yield).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08487112B2 |
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| 出典データセット | uspto-grants-2013_07 |
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| ORD ID | ord-8236c195a16443edb1720bb9f06d759e |
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| 出典メモ | uspto-grants-2013_07 |
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