HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Hydroxyurethane → 3-(3-[Ethoxycarbonylaminooxymethyl]-4-chloro-6-fluorophenyl)-1-amino-6-trifluoromethyl-1,2,3,4-tetrahydropyrimidine-2,4-dione
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Hydroxyurethane | HCID 11510 | — |
| Edukt | 1,1'-Carbonyldiimidazole | HCID 68263 | — |
| Edukt | 3-(3-Hydroxymethyl-4-chloro-6-fluorophenyl)-1-amino-6-trifluoromethyl-1,2,3,4-tetrahydropyrimidine-2,4-dione | HCID 18788057 | — |
| Lösungsmittel | Tetrahydrofuran | HCID 8028 | — |
| Produkt | 3-(3-[Ethoxycarbonylaminooxymethyl]-4-chloro-6-fluorophenyl)-1-amino-6-trifluoromethyl-1,2,3,4-tetrahydropyrimidine-2,4-dione | HCID 18788059 | — |
Reaktionsschritte
0.9 g of carbonyldiimidazole was added to a solution of 1.8 g of 3-(3-hydroxymethyl-4-chloro-6-fluorophenyl)-1-amino-6-trifluoromethyl-1,2,3,4-tetrahydropyrimidine-2,4-dione in 100 ml of tetrahydrofuran. After the reaction mixture had been stirred for 1 hour, 0.58 g of N-ethoxycarbonylhydroxylamine was added. The mixture was subsequently stirred for a further 14 hours at 20° C. whereupon the solvent was removed by distillation. The residue was taken up in 100 ml of methylene chloride. The resulting organic phase was washed with water, dried over sodium sulfate and finally concentrated. The crude product was purified by means of chromatography on silica gel (eluent: methylene chloride). Yield: 0.2 g.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US06057269 |
| Quelldatensatz | uspto-grants-2000_05 |
| ORD ID | ord-cef527b1ed174e098b6b084de0aaf99d |
| Quellennotiz | uspto-grants-2000_05 |