HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Sodium hydride → 2-(1-Pyrrolidinyl)ethyl 1-pyrrolidineacetate
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Sodium hydride | HCID 24758 | — |
| Edukt | 1-Pyrrolidineethanol | HCID 76288 | — |
| Edukt | 1-Pyrrolidineacetic acid, ethyl ester | HCID 210996 | — |
| Produkt | 2-(1-Pyrrolidinyl)ethyl 1-pyrrolidineacetate | HCID 19796137 | — |
Reaktionsbedingungen
| Temperatur | 225 °C |
|---|
Reaktionsschritte
To a mixture of 1.3 g of sodium hydride (in the form of a 60% by weight suspension in mineral oil) and 100 g (0.64 mol) of ethyl 1-pyrrolidineacetate was added 91 g of 2-(1-pyrrolidinyl)ethanol. The mixture was heated slowly to about 225° C., and the ethanol by-product was collected in a Dean-Stark trap. The reaction mixture was cooled to about 25° C., then 12 g of 1-bromopropane was added to react any alkoxide present. The sodium bromide by-product was removed by filtration. The desired product 2-(1-pyrrolidinyl)ethyl 1-pyrrolidineacetate was purified by distillation at 95° C. at a pressure of 250 μmHg. The structural assignment was confirmed by mass spectral analysis.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US05244997 |
| Quelldatensatz | uspto-grants-1993_09 |
| ORD ID | ord-c4df8ed7448a4eceb5456f490db7f354 |
| Quellennotiz | uspto-grants-1993_09 |