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Pyridine → 1-(Mesyloxymethyl)cyclohexanecarboxaldehyde
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Pyridine | HCID 1049 | — |
| 反応物 | Methanesulfonyl chloride | HCID 31297 | — |
| 反応物 | 1-(Hydroxymethyl)-cyclohexanecarboxaldehyde | HCID 13106397 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 1-(Mesyloxymethyl)cyclohexanecarboxaldehyde | HCID 22325261 | 77.8% |
反応手順
To a cold (0° C. mixture of alcohol 54 (75 g, 0.54 mole) and 65.29 g (0.57 mole) of methanesulfonyl chloride in 80 ml of methylene chloride was added a solution of pyridine (47.96 g, 0.57 mole) in 40 ml of methylene chloride. The reaction mixture was stirred at room temperature for 18 h then quenched with water, acidified with conc. HCl and extracted with methylene chloride. The organic layer was washed with water, brine, and dried over sodium sulfate and concentrated under vacuum to give 91.63 g (77.8%) of thick oil. Proton NMR and mass spectra were consistent with the product.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06943189B2 |
| 出典データセット | uspto-grants-2005_09 |
| ORD ID | ord-45dafcdbb98245a18e5c1716b6289a95 |
| 出典メモ | uspto-grants-2005_09 |