HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
1,1'-Carbonyldiimidazole → (R)-N-(5-(2-(3-chloro-5-fluorophenyl)pyrrolidin-1-yl)pyrazolo[1,5-a]pyrimidin-3-yl)-3-hydroxyazetidine-1-carboxamide
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | 1,1'-Carbonyldiimidazole | HCID 68263 | — |
| Edukt | Diisopropylethylamine | HCID 81531 | — |
| Edukt | 3-Hydroxyazetidine hydrochloride | HCID 2759290 | — |
| Edukt | (R)-5-(2-(3-chloro-5-fluorophenyl)pyrrolidin-1-yl)pyrazolo[1,5-a]pyrimidin-3-amine | HCID 67330213 | — |
| Lösungsmittel | Dichloromethane | HCID 6344 | — |
| Produkt | (R)-N-(5-(2-(3-chloro-5-fluorophenyl)pyrrolidin-1-yl)pyrazolo[1,5-a]pyrimidin-3-yl)-3-hydroxyazetidine-1-carboxamide | HCID 58386302 | 74% |
Reaktionsschritte
To a DCM (0.7 mL) solution of (R)-5-(2-(3-chloro-5-fluorophenyl)pyrrolidin-1-yl)pyrazolo[1,5-a]pyrimidin-3-amine (20 mg, 0.06 mmol, prepared as described in the following paragraph), was added CDI (20 mg, 0.12 mmol) at ambient temperature in one portion. After stirring two hours, azetidin-3-ol hydrochloride (20 mg, 0.18 mmol) was added in one portion, followed by addition of DIEA (0.032 mL, 0.18 mmol). The reaction was stirred overnight before it was concentrated and directly purified by reverse-phase column chromatography, eluting with 0 to 60% acetonitrile/water to yield the final product as a solid (29 mg, 74% yield). MS (apci) m/z=431.2 (M+H).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08865698B2 |
| Quelldatensatz | uspto-grants-2014_10 |
| ORD ID | ord-268e7b2820a24b799ff1a401ae9f774d |
| Quellennotiz | uspto-grants-2014_10 |