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Triethylamine → 1-(tert-Butoxycarbonyl)-4-(methanesulfonyloxy)piperidine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Methanesulfonyl chloride | HCID 31297 | — |
| 反応物 | Tert-butyl 4-hydroxypiperidine-1-carboxylate | HCID 643502 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 1-(tert-Butoxycarbonyl)-4-(methanesulfonyloxy)piperidine | HCID 4184869 | 98.7% |
反応手順
To a solution of 1.00 g (4.97 mmol) of N-t-butoxycarbonyl-4-hydroxypiperidine and 0.83 ml (5.96 mmol) of triethylamine in 50 ml of methylene chloride was added 0.46 ml (5.96 mmol) of methanesulfonylchloride under ice-cooling and stirring and the mixture was stirred at room temperature for 30 minutes. The reaction mixture was washed with an aqueous saturated sodium bicarbonate solution and water and dried. The solvent was distilled off. The residue was washed with hexane to obtain 1.37 g of the desired compound (98.6%, colorless powder), mp: 87.0°-88.0° C.
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-7030c1fd7e86451f857a9e61a4bc804b |
| 出典メモ | uspto-grants-1993_09 |