HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Ethanol → 1,4-Dioxa-10-azadispiro[4.2.4.2]tetradecan-9-one
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Ethanol | HCID 702 | — |
| Edukt | Ethyl 2-(8-(nitromethyl)-1,4-dioxaspiro[4.5]decan-8-yl)acetate | HCID 59505535 | — |
| Katalysator | Nickel | HCID 935 | — |
| Produkt | 1,4-Dioxa-10-azadispiro[4.2.4.2]tetradecan-9-one | HCID 58230108 | 83,8% |
Reaktionsschritte
To a solution of ethyl 2-(8-(nitromethyl)-1,4-dioxaspiro[4.5]decan-8-yl)acetate (109 g, 379.38 mmol) in EtOH (600 mL) was added Raney Ni (10 g). The reaction mixture was stirred under H2 atmosphere at rt for 72 h and filtered. The filter cake was washed with a mixture of DCM and MeOH (1/1 (v/v), 500 mL). The filtrated was concentrated in vacuo and the residue was washed with a mixture of PE and EtOAc (10/1 (v/v), 800 mL) and filtered to give the product as a white solid (67 g, 83.8%).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US09399637B2 |
| Quelldatensatz | uspto-grants-2016_07 |
| ORD ID | ord-3514c8bcf6604b48a6e06ff04d1e7fe6 |
| Quellennotiz | uspto-grants-2016_07 |