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Dimethylformamide → Methyl 2-chloro-6-methylpyridine-3-carboxylate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Dimethylformamide | HCID 6228 | — |
| 反応物 | Oxalyl chloride | HCID 65578 | — |
| 反応物 | 2-Chloro-6-methylnicotinic acid | HCID 121724 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | Methyl 2-chloro-6-methylpyridine-3-carboxylate | HCID 13055804 | — |
反応手順
To a suspension of 2-chloro-6-methylnicotinic acid (5.3 g, 30.8 mmol) in dichloromethane (100 ml) at 0° C. were added DMF (1 ml) and oxalyl chloride (3.2 ml, 36.9 mmol). The mixture was allowed to warmn to room temperature and stirred for 5 h. The solvents were removed in vacuo and the residue was dissolved in dichloromethane (50 ml) and methanol (50 ml). The mixture was stirred at room temperature for 18 h and then concentrated in vacuo. The residue was dissolved in chloroform, washed with saturated sodium bicarbonate solution and brine, dried over MgSO4, and concentrated in vacuo to give a brown oil; yield 5.70 g (100%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07176195B2 |
| 出典データセット | uspto-grants-2007_02 |
| ORD ID | ord-e8a38c9878e446839eb2daf1c59b6e4a |
| 出典メモ | uspto-grants-2007_02 |