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Potassium Carbonate → Methyl 2-((5-methoxy-6-nitropyridin-2-yl)methylthio)acetate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 3-Methoxy-2-nitro-6-pyridylmethyl bromide | HCID 14405124 | — |
| 反応物 | 2-Mercaptopropionate | HCID 15607736 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | Methyl 2-((5-methoxy-6-nitropyridin-2-yl)methylthio)acetate | HCID 67994824 | — |
反応手順
A mixture of 6-(bromomethyl)-3-methoxy-2-nitropyridine (30 mmol, 0.74 g), methythioglycolate (2.7 mL, 30 mmol), and potassium carbonate (5.5 g, 40 mmol) in methanol (200 mL) was stirred at room temperature for 10 hours. After concentrated the mixture was purified by column chromatography using PE/DCM (1:1, v/v) followed by DCM to the titled compound. 1H-NMR (CDCl3): δ 3.27 (S, 2H, CH2), 3.74 (S, 3H, OCH3), 3.93 (S, 2H, CH2), 3.99 (S, 3H, OCH3), 7.51 (d, 1H, J=8.6 Hz, Py-H), 7.65 (d, 1H, J=8.6 Hz, Py-H); HR-MS (ESI+) m/z 272.0467 [M+H]+ C10H12N2O5S requires 273.0547.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08829003B2 |
| 出典データセット | uspto-grants-2014_09 |
| ORD ID | ord-41f55f15631d41559d11993553177430 |
| 出典メモ | uspto-grants-2014_09 |