HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
2,2,2-Trifluoroethylhydrazine → 3,3a,4,5,6,7-hexahydro-3-phenyl-7-(phenylmethylene)-2-(2,2,2-trifluoroethyl)-2H-pyrazolo[4,3-c]-pyridine, monohydrochloride
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | 2,2,2-Trifluoroethylhydrazine | HCID 78740 | — |
| Edukt | 4-Piperidinone, 3,5-bis(phenylmethylene)-, hydrochloride | HCID 355749 | — |
| Lösungsmittel | Methanol | HCID 887 | — |
| Produkt | 3,3a,4,5,6,7-hexahydro-3-phenyl-7-(phenylmethylene)-2-(2,2,2-trifluoroethyl)-2H-pyrazolo[4,3-c]-pyridine, monohydrochloride | HCID 131710993 | 107% |
Reaktionsschritte
3,5-Dibenzylidene-4-piperidone, hydrochloride (10.0g) is reacted with 5.8 g of 70% aqueous 2,2,2-trifluoroethylhydrazine in 220 ml of methanol at reflux for 4 hours. Evaporation of the methanol on a rotary evaporator leaves 14 g of a foamy residue which crystallizes when triturated with 50 ml of boiling acetonitrile to yield (after cooling for about 16 hours) 10.3 g of material, melting point 206°-209° C (sintering at 195° C). Crystallization from 80 ml of ethanol yields 6.7 g of product, melting point 207°-209° C, sintering at 196° C.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US04065617 |
| Quelldatensatz | uspto-grants-1977_12 |
| ORD ID | ord-c6ed15a73c8940a9a85cad248df3f631 |
| Quellennotiz | uspto-grants-1977_12 |