HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
1,2-Dichloroethane → Isobutyric acid N'-(5-fluoro-pyridin-2-yl)-hydrazide
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | 1,2-Dichloroethane | HCID 11 | — |
| Edukt | Isobutyric Acid | HCID 6590 | — |
| Edukt | Sodium Bicarbonate | HCID 516892 | — |
| Edukt | 1-Hydroxybenzotriazole hydrate | HCID 2796029 | — |
| Edukt | 5-Fluoro-2-hydrazinylpyridine | HCID 19916786 | — |
| Lösungsmittel | Dichloromethane | HCID 6344 | — |
| Produkt | Isobutyric acid N'-(5-fluoro-pyridin-2-yl)-hydrazide | HCID 66977821 | 46% |
Reaktionsschritte
A solution of 5-fluoro-2-hydrazinyl-pyridine (0.59 g, 4.65 mmol), isobutyric acid (528 mg, 6 mmol), and HOBt hydrate (153 mg, 1 mmol) in DCM (10 mL) was treated with EDC (1.15 g, 6 mmol). The reaction mixture was stirred at RT for 40 min, poured onto sat. aq. sodium bicarbonate (40 mL), extracted with four portions of DCM, dried (Na2SO4), evaporated and purified by FCC using 10-30% EtOAc/DCM to give the title compound (0.42 g, 46%). LCMS (method 2): Rt 2.46 min, m/z 198 [MH+].
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08916708B2 |
| Quelldatensatz | uspto-grants-2014_12 |
| ORD ID | ord-f64fbdcf1c55469ca59147b1d94fad71 |
| Quellennotiz | uspto-grants-2014_12 |