関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | 4-Piperidinecarboxylic acid | HCID 3773 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Carbonic acid, bis(1,1-dimethylethyl) ester | HCID 10219638 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | 1-(tert-Butoxycarbonyl)-4-piperidinecarboxylic acid | HCID 392871 | 95.8% |
反応手順
8.6 g of triethylamine and 20 ml of water are added to a solution of 10 g of isonipecotic acid in 100 ml of dioxane and the mixture is heated to 60° C. 20.25 g of di-tert-butyl carbonate are then added dropwise and the mixture is stirred for 1 hour at 60° C. and refluxed for 30 minutes. It is concentrated under vacuum, the residue is taken up with water and acidified to pH 3 by the addition of 2 N HCl solution and the precipitate formed is filtered off to give 17 g of the expected product.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US06710042B2 |
|---|
| 出典データセット | uspto-grants-2004_03 |
|---|
| ORD ID | ord-2839b4b8535f4f1284e5c5ef0171095d |
|---|
| 出典メモ | uspto-grants-2004_03 |
|---|
