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-chloromethylthiazole | HCID 2763179 | — |
| 反応物 | 4-(benzylamino)furan-2(5H)-one | HCID 13402453 | — |
| 溶媒 | 1,2-Dimethoxyethane | HCID 8071 | — |
| 生成物 | 4-{benzyl[(2-chloro-1,3-thiazol-5-yl)methyl]amino}furan-2(5H)-one | HCID 68489197 | 71% |
反応手順
6.3 g of 4-(benzylamino)furan-2(5H)-one (Example 16) are initially charged in 75 ml of dimethoxyethane at room temperature. Subsequently, 1.3 g of sodium hydroxide are added and, at 40° C., 34.4 g of a 15% solution of 2-chloro-5-(chloromethyl)-1,3-thiazole 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 50 ml of water and 50 ml of methylene chloride. The organic phase is removed, and the aqueous phase is extracted once again with 50 ml of methylene chloride. The combined methylene chloride phases are dried over sodium sulphate and the solvent is removed under reduced pressure. 6.9 g of 4-{benzyl[(2-chloro-1,3-thiazol-5-yl)methyl]amino}furan-2(5H)-one are obtained (this corresponds to 71% 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-21a7e2cd56fd4ac88c4bb560daf0bd29 |
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| 出典メモ | uspto-grants-2013_07 |
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