関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Benzyl chloroformate | HCID 10387 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | 4-Piperidinecarboxylic acid, 4-phenyl-, 4-methylbenzenesulfonate (1:1) | HCID 2723657 | — |
| 溶媒 | Acetone | HCID 180 | — |
| 生成物 | 1-(Benzyloxycarbonyl)-4-phenylpiperidine-4-carboxylic acid | HCID 22741798 | 90.3% |
反応手順
A mixture of 37.7 g of 4-carboxy-4-phenylpiperidine p-toluenesulphonate, 53.3 g of 30% aqueous NaOH solution and 250 ml of water is cooled to 5° C. A solution of 18 g of benzyl chloroformate in 60 ml of acetone is added rapidly at 5° C., and the mixture is left stirring overnight while allowing the temperature to rise to RT. The reaction mixture is washed twice with ether and, after settling has taken place, the aqueous phase is separated and acidified to pH 1 by adding concentrated HCl and then 2N HCl. The precipitate formed is drained, dried, taken up in ether and drained again. 30.6 g of the expected product are obtained, m.p.=142°-144° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US05830906 |
|---|
| 出典データセット | uspto-grants-1998_11 |
|---|
| ORD ID | ord-9edd3216b4c04336a113c215dc3d42bf |
|---|
| 出典メモ | uspto-grants-1998_11 |
|---|
