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2,6-Dichloro-4-nitropyridine → 2,6-Dichloro-4-(methylthio)pyridine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 2,6-Dichloro-4-nitropyridine | HCID 3841070 | — |
| 反応物 | Sodium methanethiolate | HCID 4378561 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 2,6-Dichloro-4-(methylthio)pyridine | HCID 18950231 | 74.7% |
反応手順
To a solution of 2,6-dichloro-4-nitropyridine (3.8 g; 0.02 mol) in dimethylformamide (50 ml) cooled with an ice-bath was sodium thiomethoxide (1.4 g; 0.02 mol) slowly added. After stirring for 3 hours, the reaction mixture was quenched with water (300 ml) and extracted 3 times each with a hexane/ethyl acetate mixture (100 ml; 1/1). The combined extracts were dried with anhydrous magnesium sulphate and the solvent was removed in vacuo. Purification by silica gel flash column chromatography afforded 2,6-dichloro-4-methylthiopyridine (2.9 g; 74%) as a colorless oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05374604 |
| 出典データセット | uspto-grants-1994_12 |
| ORD ID | ord-7eadde4d1ac241ffbff21fb1c8f76752 |
| 出典メモ | uspto-grants-1994_12 |