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Benzylamine → 4-[3-(N-benzylamino)propylthio)pyridine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Benzylamine | HCID 7504 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Methanesulfonyl chloride | HCID 31297 | — |
| 反応物 | 4-(3-Hydroxypropylthio)pyridine | HCID 19079134 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 4-[3-(N-benzylamino)propylthio)pyridine | HCID 19079190 | 16.1% |
反応手順
In 150 ml of methylene chloride were dissolved 5.22 g (30.8 mmol) of 4-(3-hydroxypropylthio)pyridine and 5.16 ml (37.0 mmol) of triethylamine, methanesulfonyl chloride [2.86 ml (37.0 mmol)] was added, and 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. Then the solvent was distilled off. 2.62 ml (24.0 mmol) of benzylamine was added to the residue, and the mixture was heated at 80° C. for 3 hours. After cooling, the mixture was purified by column chromatography (eluent: chloroform /methanol=25:1) to obtain 1.0 g of the desired compound (yield: 16.1%, 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-cead92d510b44868b7a17bfdcce47e62 |
| 出典メモ | uspto-grants-1993_09 |