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Acetyl chloride → 4-[3-(N-2-pyridylmethyl-N-acetylamino)propylthio]pyridine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Acetyl chloride | HCID 6367 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 4-(3-(N-2-pyridylmethylamino)propylthio]pyridine | HCID 19079176 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 4-[3-(N-2-pyridylmethyl-N-acetylamino)propylthio]pyridine | HCID 19079165 | 85.6% |
反応手順
To a solution of 1.62 g (6.24 mmol) of 4-[3-(N-2pyridylmethylamino)propylthio]pyridine and 1.10 ml (7.80 mmol) of triethylamine in 10 ml of methylene chloride, 0.51 ml (7.80 mmol) of acetyl chloride was added under ice-cooling with stirring. The mixture was stirred at room temperature for 30 minutes. The reaction mixture was washed with a saturated aqueous solution of sodium bicarbonate and water and dried, and the solvent was distilled off. The residue was purified by column chromatography (eluent: ethyl acetate/methanol=10:1) to obtain 1.61 g of the desired compound (yield: 85.6%, yellow oil).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05246948 |
| 出典データセット | uspto-grants-1993_09 |
| ORD ID | ord-c1f38a3c62784772a0ad020614ddd68f |
| 出典メモ | uspto-grants-1993_09 |