関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Morpholine | HCID 8083 | — |
| 反応物 | 6-Bromo-2-methyl-3-nitropyridine | HCID 24728014 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 4-(6-Methyl-5-nitro-2-pyridinyl)morpholine | HCID 8208955 | 69.7% |
反応手順
To a solution of 6-bromo-2-methyl-3-nitropyridine (2.05 g, 9.45 mmol) in ethanol (10 mL) was added morpholine (1.728 mL, 19.84 mmol) and the reaction mixture was stirred at 70° C. for 5 hours. The reaction mixture was allowed to cool to room temperature causing a precipitate. The solid was collected by filtration and washed with ethanol (5 mL), then dried in vacuo. The crude was redissolved in a mixture of saturated sodium carbonate solution and ethyl acetate. The organic phase was separated, washed with further saturated sodium carbonate solution, then dried over magnesium sulphate and evaporated in vacuo to give the title compound (1.47 g) as a yellow solid. LCMS (2 min, formic) Rt 0.92 min, m/z (ES+) 224 (M+H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09242972B2 |
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| 出典データセット | uspto-grants-2016_01 |
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| ORD ID | ord-456d0803c97f4b36b810f7a4623636de |
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| 出典メモ | uspto-grants-2016_01 |
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