関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | N-(2-Aminoethyl)piperidine | HCID 33944 | — |
| 反応物 | Tetrahydrophthalic anhydride, cis- | HCID 98495 | — |
| 反応物 | Sodium borohydride | HCID 4311764 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Isopropanol | HCID 3776 | — |
| 生成物 | 6-(Hydroxymethyl)-N-(2-piperidinoethyl)-3-cyclohexene-1-carboxamide | HCID 21266117 | — |
反応手順
N-(2-Aminoethyl)piperidine (2.11 g) was added to cis-4-cyclohexene-1,2-dicarboxylic anhydride (2.50 g) and stirred for 6 hours at 140° C. The reaction mixture was suspended into a mixed solution of 2-propanol (125 ml) and water (21 ml) and then sodium borohydride (3.12 g) was added thereto at room temperature. After being stirred for 68 hours at room temperature, the reaction mixture was acidified with dilute hydrochloric acid and then concentrated. The residue was adjusted to pH 9 with saturated sodium hydrogencarbonate aqueous solution and 1N sodium hydroxide, and then extracted with ethyl acetate. The extract was washed with saturated brine, dried over sodium sulfate anhydride, and concentrated, thereby yielding a crude (3.34 g) containing the entitled compound as brown syrup.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06174885B1 |
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| 出典データセット | uspto-grants-2001_01 |
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| ORD ID | ord-c1fd2ea043c24870adbe68e0b74e7971 |
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| 出典メモ | uspto-grants-2001_01 |
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