HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
4-Piperidinecarboxylic acid → 1-Carbobenzoxy-4-piperidinecarboxylic Acid
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | 4-Piperidinecarboxylic acid | HCID 3773 | — |
| Edukt | Benzyl chloroformate | HCID 10387 | — |
| Edukt | Sodium Hydroxide | HCID 14798 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Produkt | 1-Carbobenzoxy-4-piperidinecarboxylic Acid | HCID 736489 | 91,2% |
Reaktionsbedingungen
| Temperatur | 0 °C |
|---|
Reaktionsschritte
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]+.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08841278B2 |
| Quelldatensatz | uspto-grants-2014_09 |
| ORD ID | ord-fb9c46f13c284be7a5dbf978b5db7cdc |
| Quellennotiz | uspto-grants-2014_09 |