HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Triethylamine → 2-[2-(4-Cyclopropyl-phenyl)-1-oxo-2,8-diaza-spiro[4.5]dec-8-yl]-propionic acid
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Triethylamine | HCID 8471 | — |
| Edukt | 2-Bromopropionic acid | HCID 11729 | — |
| Edukt | 2-(4-Cyclopropyl-phenyl)-2,8-diaza-spiro[4.5]decan-1-one | HCID 58287277 | — |
| Lösungsmittel | 1,2-Dichloroethane | HCID 11 | — |
| Produkt | 2-[2-(4-Cyclopropyl-phenyl)-1-oxo-2,8-diaza-spiro[4.5]dec-8-yl]-propionic acid | HCID 58287264 | 19,5% |
Reaktionsbedingungen
| Temperatur | 80 °C |
|---|
Reaktionsschritte
A mixture of 200 mg (0.74 mmol) 2-(4-Cyclopropyl-phenyl)-2,8-diaza-spiro[4.5]decan-1-one, 168 mg (1.11 mmol) 2-bromo-propionic acid and 224 mg (2.21 mmol) NEt3 in 5 mL DCE was heated to 80° C. for 2 h and concentrated. The residue was taken up in methanol and subjected to purification by preparative HPLC on reversed phase eluting with a gradient formed from acetonitrile, water and formic acid. The product containing fractions were evaporated to yield 49.4 mg (19%) of the title compound. MS m/e: 343.2 [M+H]+.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08389539B2 |
| Quelldatensatz | uspto-grants-2013_03 |
| ORD ID | ord-79ec2db2d21842a599b263b97595fa8c |
| Quellennotiz | uspto-grants-2013_03 |