HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Ethyl Acetate → HCID 68784889, Verbindung
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Ethyl Acetate | HCID 8857 | — |
| Edukt | Sodium hydride | HCID 24758 | — |
| Edukt | 1-(3-Chloro-propyl)-3-(4-methyl-pyridin-3-yl)-urea | HCID 68786992 | — |
| Lösungsmittel | Dimethylformamide | HCID 6228 | — |
| Lösungsmittel | Tetrahydrofuran | HCID 8028 | — |
| Produkt | HCID 68784889 | HCID 68784889 | 96,5% |
Reaktionsschritte
1-(3-Chloro-propyl)-3-(4-methyl-pyridin-3-yl)-urea (I-130a: 2 g, 9.25 mmol) in dry DMF (15 mL) was added to a stirred mixture of sodium hydride (330 mg, 13.87 mmol) in THF (30 mL) at 0° C. The reaction was stirred at room temperature for 1 hour. The reaction was monitored by TLC (100% ethylacetate). The reaction mixture was quenched with MeOH at 0° C., concentrated under reduced pressure and partitioned between ice water and chloroform. The organic layer was washed with brine solution, dried over Na2SO4 and concentrated under reduced pressure to afford 1.7 g (96.5% yield) of 1-(4-methyl-pyridin-3-yl)-tetrahydro-pyrimidin-2-one.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08263635B2 |
| Quelldatensatz | uspto-grants-2012_09 |
| ORD ID | ord-90e862bc69a344388e22a43af32a1fd1 |
| Quellennotiz | uspto-grants-2012_09 |