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Water → 1,2-bis[N-[4-(4-pyridylthio)butyl]-N-propionylamino]benzene
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Potassium Hydroxide | HCID 14797 | — |
| 反応物 | 1,2-bis[N-(4-chlorobutyl)-N-propionylamino]benzene | HCID 19079254 | — |
| 反応物 | pyridine-4-thiol | HCID 178418431 | — |
| 溶媒 | Dimethyl Sulfoxide | HCID 679 | — |
| 生成物 | 1,2-bis[N-[4-(4-pyridylthio)butyl]-N-propionylamino]benzene | HCID 19079128 | 81% |
反応手順
To a solution of 525 mg (4.7 mmol) of 4-mercaptopyridine and 265 mg (4.7 mmol) of potassium hydroxide in 20 ml of dimethyl sulfoxide, 760 mg (1.89 mmol) of 1,2-bis[N-(4-chlorobutyl)-N-propionylamino]benzene was added at room temperature, and the mixture was stirred for 2 hours. The reaction mixture was poured into water and the mixture was extracted with ethyl acetate. The extract was dried and the solvent was distilled off. The residue was purified by column chromatography (eluent: ethyl acetate to ethyl acetate/ethanol =20:1 to 10:1 to 5:1) to give 0.84 g of the desired product (81.0% yield, pale yellow crystals).
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-037000249bf248819c335444fe0d73ae |
| 出典メモ | uspto-grants-1993_09 |