HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Triethylamine → 1-[9-(prop-2-en-1-yl)-6-oxaspiro[4.5]decan-9-yl]-1H-pyrazole
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Triethylamine | HCID 8471 | — |
| Edukt | 3-(Dimethylamino)-2-propenal | HCID 79125 | — |
| Edukt | [9-(Prop-2-en-1-yl)-6-oxaspiro[4.5]decan-9-yl]hydrazine | HCID 68314598 | — |
| Lösungsmittel | Isopropanol | HCID 3776 | — |
| Produkt | 1-[9-(prop-2-en-1-yl)-6-oxaspiro[4.5]decan-9-yl]-1H-pyrazole | HCID 68314165 | 31% |
Reaktionsschritte
A solution of [9-(prop-2-en-1-yl)-6-oxaspiro[4.5]decan-9-yl]hydrazine (250 mg, 1.0 mmol) in 4 mL of i-PrOH were added Et3N and 3-dimethylaminoacrolein. The solution was refluxed for 3 h and then at 50° C. for 2 d. The solvent removed and the residue was purified on 25 g Biotage snap column, eluted with 0-18% EtOAc in Hex (12 CV) to give 1-[9-(prop-2-en-1-yl)-6-oxaspiro[4.5]decan-9-yl]-1H-pyrazole (80 mg, 31% yield).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08835488B2 |
| Quelldatensatz | uspto-grants-2014_09 |
| ORD ID | ord-a605260e4fe14622971415496bbdd4f6 |
| Quellennotiz | uspto-grants-2014_09 |