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 | Ethyl 4-hydroxypiperidine-1-carboxylate | HCID 96394 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 1-Ethoxycarbonyl-4-methyloxypiperidine | HCID 45120191 | — |
反応手順
1-ethoxycarbonyl-4-hydroxypiperidine (30.3 g) and triethylamine (23 g) were dissolved in ethyl acetate (182 mL) and the obtained mixture was cooled to 3° C. Methanesulfonyl chloride (22.05 g) was added thereto under stirring while taking caution such that the temperature did not exceed 20° C., and the mixture was continuously stirred under ice cooling for 1 hour. The obtained reaction mixture was washed with water (90 mL×3). The organic layer was isolated and concentrated to obtain a target compound as a light yellow oily substance. The yield amount was 43.09 g (98%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08552188B2 |
|---|
| 出典データセット | uspto-grants-2013_10 |
|---|
| ORD ID | ord-46653c60c6b244bfafb34f1aaeb28f08 |
|---|
| 出典メモ | uspto-grants-2013_10 |
|---|
