関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Cyclohexylmethane sulfonyl chloride | HCID 3871475 | — |
| 反応物 | methyl (2S)-piperidine-2-carboxylate hydrochloride | HCID 13246232 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | HCID 57106621 | HCID 57106621 | 70.5% |
反応手順
Triethylamine (22.15 ml) was added to a solution of (2S)-2-(methoxycarbonyl)piperidine hydrochloride (10 g) [see Preparation 24] and cyclohexylmethanesulfonyl chloride (16.42 g) [King. J. F. et al,. J. Am. Chem. Soc., 1992, 114(5), 1743-9] in dichloromethane (100 ml). The reaction mixture was stirred for 18 hours after which time the solvent was removed under reduced pressure and the residue diluted with ethyl acetate. The organic layer was washed with water, brine, dried over magnesium sulphate and the solvent was removed under reduced pressure. The crude product was purified by column chromatography on silica gel eluting with a solvent gradient of 95:5 changing to 80:20, by volume, hexane:ethyl acetate to afford methyl (2S)-1-[(cyclohexylmethyl)sulfonyl]-2-piperidinecarboxylate (11.9 g) as a white solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US06610707B1 |
|---|
| 出典データセット | uspto-grants-2003_08 |
|---|
| ORD ID | ord-8fae7256d29a449793106bcdde891b9f |
|---|
| 出典メモ | uspto-grants-2003_08 |
|---|