HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
4-Piperidinecarboxylic acid → 1,1'-[Dithiobis(2,1-phenylenecarbonyl)]bis-4-piperidine carboxylic acid
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | 4-Piperidinecarboxylic acid | HCID 3773 | — |
| Edukt | N-Trimethylsilyl-N-methylacetamide | HCID 81953 | — |
| Edukt | 2,2'-Dithiodibenzoyl chloride | HCID 88164 | — |
| Katalysator | Pyridine | HCID 1049 | — |
| Lösungsmittel | Dichloromethane | HCID 6344 | — |
| Produkt | 1,1'-[Dithiobis(2,1-phenylenecarbonyl)]bis-4-piperidine carboxylic acid | HCID 18935289 | — |
Reaktionsschritte
Isonipecotic acid (4-piperidinecarboxylic acid) (0.76 g, 6 mmol), N-methyl-N-trimethylsilylacetamide and 3 drops of pyridine were stirred at room temperature for 2 hours. This suspension was added to a filtered solution of 2,2'-dithiobisbenzoyl chloride (1.0 g, 3.0 mmol) in 15 mL of dichloromethane. The solvent was removed after 18 hours and the residue was triturated with 1N HCl. The acid was decanted and the residue was dissolved in acetonitrile. After standing for 24 hours a precipitate formed. The solid was collected and dried to give 0.56 g of the title compound, mp>250° C.;
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US05734081 |
| Quelldatensatz | uspto-grants-1998_03 |
| ORD ID | ord-90022719d27c459586f6b49166817b5d |
| Quellennotiz | uspto-grants-1998_03 |