関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | N-Aminomorpholine | HCID 20315 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | 1-Hydroxybenzotriazole hydrate | HCID 2796029 | — |
| 反応物 | 2-Hydroxy-2-phenyl-2-(3-pyridinyl)acetic acid | HCID 10561376 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | 2-Hydroxy-N-(4-morpholinyl)-2-phenyl-2-(3-pyridinyl)-acetamide | HCID 9948709 | 83.4% |
反応手順
A mixture of 2-hydroxy-2-phenyl-2-(3-pyridinyl)acetic acid (3.48 g, 0. 015 mole) , 1-hyrdoxybenzotriazole hydrate (4.10 g, 0.03 mole), 1,3-Dicyclohexycarbodiimide (3.09 g, 0.015 mole), 4-aminomorpholine (1.45 ml, 0.015 mole), sodium bicarbonate (1.26 g, 0.015 mole), N,N-dimethyformamide (36 ml) and dioxane (36 ml) were stirred at room temperature overnight. The volatiles were removed in vacuo, dichloromethane (170 ml) was added and following filtration, the organic layer was washed with saturated sodium bicarbonate and brine. After drying, filtration and concentration, the residue was purified by column chromatography using 10% methanol in chloroform to give 3.92 g of the product as a white foam. High Res. Mass Spec. Calcd. for C17H19N3O3 :314.1505 (M+H). Found: 314.1501.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05428035 |
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| 出典データセット | uspto-grants-1995_06 |
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| ORD ID | ord-eb69e07ce28f4f7c848e864fd55145cd |
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| 出典メモ | uspto-grants-1995_06 |
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