HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Sodium Carbonate → 1-(Tetrahydro-2-furoyl)piperazine
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Sodium Carbonate | HCID 10340 | — |
| Edukt | Sodium Hydroxide | HCID 14798 | — |
| Edukt | 1-(2-Furoyl)piperazine | HCID 550206 | — |
| Edukt | 1-(2-Tetrahydrofuroyl)piperazine hydrobromide | HCID 16217252 | — |
| Katalysator | Nickel | HCID 935 | — |
| Lösungsmittel | Methanol | HCID 887 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Produkt | 1-(Tetrahydro-2-furoyl)piperazine | HCID 2734641 | — |
Reaktionsschritte
The furoylpiperazine of Example 1 was converted to the hydrobromide salt (m.p. 173°-175° C.). This salt (39.0 g) in 250 ml methyl alcohol and 9.0 g Raney nickel was hydrogenated at 3 atm. After uptake of H2 ceased, the catalyst was filtered, the solvent concentrated, and the residue crystallized from isopropyl alcohol to give 35.2 g. tetrahydrofuroylpiperazine HBr, m.p. 152°-156° C. This was suspended in 20 ml H2O. Then 10.5 g 50%, NaOH solution was added slowly followed by 2.0 g solid Na2CO3. This was extracted with 4×100 ml portions of warm CHCl3. The CHCl3 extractions were distilled to give 22.5 g tetrahydrofurolylpiperazine, b.p. 120°-125° C./0.2 mm Hg.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US05861309 |
| Quelldatensatz | uspto-grants-1999_01 |
| ORD ID | ord-0ce1210b61264f4391e1f370710c5052 |
| Quellennotiz | uspto-grants-1999_01 |