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Methanol → Pyridine, 2-(methylthio)-3-nitro-
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methanol | HCID 887 | — |
| 反応物 | 2-Chloro-3-nitropyridine | HCID 79613 | — |
| 反応物 | Sodium methanethiolate | HCID 4378561 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | Pyridine, 2-(methylthio)-3-nitro- | HCID 572042 | 64% |
反応手順
A methanol (50 ml) solution of 2-chloro-3-nitropyridine (4.30 g, 27.1 mmol) was added dropwise to a methanol (30 ml) solution of sodium thiomethoxide (2.10 g, 28.5 mmol) while being cooled with ice, and the mixed solution was stirred for 17 hours. Water was then added to the reaction mixture, and the resulting mixture was extracted with ethyl acetate. The organic layer was washed with a saturated aqueous solution of sodium chloride, and dried over sodium sulfate. Subsequently, the solvent was distilled off, and the resulting crystals were recrystallized from a mixture of an ethyl acetate-hexane mixture to obtain 2.93 g (yield 64%) of 2-methylthio-3-nitropyridine as a yellow needle crystal.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07393866B2 |
| 出典データセット | uspto-grants-2008_07 |
| ORD ID | ord-d201babce6fd40b5b66d602459b221be |
| 出典メモ | uspto-grants-2008_07 |