HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Tert-Butylamine → HCID 66661120, Verbindung
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Tert-Butylamine | HCID 6385 | — |
| Edukt | Triethylamine | HCID 8471 | — |
| Edukt | Propylphosphonic anhydride | HCID 111923 | — |
| Edukt | 4-Methylpyridine-2-carboxylic acid | HCID 2762820 | — |
| Lösungsmittel | Dichloromethane | HCID 6344 | — |
| Produkt | HCID 66661120 | HCID 66661120 | 53,6% |
Reaktionsschritte
4-Methylpyridine-2-carboxylic acid (500 mg, 3.65 mmol), triethylamine (1.27 g, 12.5 mmol, 1.75 mL) and tert-butylamine (267 mg, 3.65 mmol) were combined and stirred in dichloromethane (1 mL). 1-Propanephosphonic acid cyclic anhydride (4.82 g, 7.5 mmol, 4.5 mL, 50% solution in ethyl acetate) was added dropwise and the reaction stirred at room temperature for 1 hour. The reaction mixture was concentrated at reduced pressure and the resulting residue taken up in ethyl acetate and washed with saturated sodium bicarbonate solution. The organic phase was dried over sodium sulfate and concentrated under vacuum to afford the title compound (376 mg). MS (ESI) m/z 193.4 [M+H]+
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08759352B2 |
| Quelldatensatz | uspto-grants-2014_06 |
| ORD ID | ord-56b48c9a327b4901b2f453bf902d264d |
| Quellennotiz | uspto-grants-2014_06 |