関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 4-Piperidinecarboxylic acid | HCID 3773 | — |
| 反応物 | Benzyl chloroformate | HCID 10387 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 1-Carbobenzoxy-4-piperidinecarboxylic Acid | HCID 736489 | 91.2% |
反応手順
Piperidine-4-carboxylic acid (64.8 g, 0.5 mol) in H2O (50 mL) was treated with NaOH (44.0 g, 1.1 mol). The reaction mixture was cooled to 0° C. and treated with CbzCl (93.8 g, 0.55 mol). The reaction mixture was stirred at ambient temperature for 4 hours and the mixture was extracted with Et2O (3 150 mL). The aqueous phase was acidified with 6 N HCl (140 mL) and extracted with EtOAc (3 200 mL). The solution was dried over MgSO4, filtered, and concentrated to afford crude piperidine-1,4-dicarboxylic acid monobenzyl ester (120 g), which was used without further purification: MS (ESI) m/z 262 [M−H]+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08841278B2 |
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| 出典データセット | uspto-grants-2014_09 |
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| ORD ID | ord-fb9c46f13c284be7a5dbf978b5db7cdc |
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| 出典メモ | uspto-grants-2014_09 |
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