HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Ammonia → tert-Butyl (3R)-3-(aminomethyl)pyrrolidine-1-carboxylate
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Ammonia | HCID 222 | — |
| Edukt | (R)-1-Boc-3-cyanopyrrolidine | HCID 7018344 | — |
| Katalysator | Nickel | HCID 935 | — |
| Lösungsmittel | Ethanol | HCID 702 | — |
| Produkt | Ammonia | HCID 222 | — |
| Produkt | tert-Butyl (3R)-3-(aminomethyl)pyrrolidine-1-carboxylate | HCID 1515152 | 195,3% |
Reaktionsschritte
A mixture of tert-butyl (3R)-3-cyano-1-pyrrolidinecarboxylate (preparation 79) (1.60 g, 8.13 mmol) and Raney® Nickel (1 g) in 0.88 ammonia (20 ml) and ethanol (150 ml), was hydrogentaed at 60 psi and room temperature for 8 hrs. The mixture was filtered through Arbocel®, and the filtrate concentrated under reduced pressure. The crude product was purified by column chromatography on silica gel using an elution gradient of dichloromethane:methanol:0.88 ammonia (100:0:0 to 90:10:1) to yield the desired product as an oil, (1.59 g, 98%).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US06180627B2 |
| Quelldatensatz | uspto-grants-2001_01 |
| ORD ID | ord-1c7a07d975f346d390c3f0a0a6b4b0eb |
| Quellennotiz | uspto-grants-2001_01 |