HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Ethyl isocyanatoacetate → N-(3-aminosulfonyl-4-chloro-2-hydroxyphenyl)-N'-(ethoxycarbonyl)methylurea
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Ethyl isocyanatoacetate | HCID 76283 | — |
| Edukt | 3-Amino-6-chloro-2-hydroxy-benzenesulfonamide | HCID 11368059 | — |
| Lösungsmittel | Dimethylformamide | HCID 6228 | — |
| Lösungsmittel | Ethyl Acetate | HCID 8857 | — |
| Produkt | N-(3-aminosulfonyl-4-chloro-2-hydroxyphenyl)-N'-(ethoxycarbonyl)methylurea | HCID 10154964 | 7,5% |
Reaktionsschritte
A solution of 3-amino-6-chloro-2-hydroxybenzenesulfonamide (170 mg, 0.76 mmol) and ethyl isocyanatoacetate (103 μL, 0.92 mmol) in 1.5 mL of N,N-dimethyl-formamide was stirred at room temperature for 20 hours. The mixture was diluted with ethyl acetate and washed with water to give the crude. Purification upon column chromatograph on silica gel, eluting with ethyl acetate/hexane (60/40, v/v), followed by Gilson HPLC separation, gave the desired product (20 mg, 7%). LC-MS (m/z) 352.0 (M+).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US06767922B2 |
| Quelldatensatz | uspto-grants-2004_07 |
| ORD ID | ord-f2518a3388a049b690f3d2beba0e13ec |
| Quellennotiz | uspto-grants-2004_07 |