HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Hydrochloric Acid → HCID 178477340, Verbindung
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Hydrochloric Acid | HCID 313 | — |
| Edukt | S-Ethylisothiourea | HCID 5139 | — |
| Edukt | Ethyl Propionate | HCID 7749 | — |
| Edukt | Ethyl formate | HCID 8025 | — |
| Edukt | Sodium Methoxide | HCID 10942334 | — |
| Lösungsmittel | Methanol | HCID 887 | — |
| Lösungsmittel | Dimethylformamide | HCID 6228 | — |
| Produkt | HCID 178477340 | HCID 178477340 | 13,5% |
Reaktionsschritte
To a solution of ethyl propionate (1.2 mL, 10 mmol) in DMF (1 mL) was added sodium methoxide (740 mg, 13 mmol), and to this was added ethyl formate (560 μL, 6.7 mmol) very slowly over 1 h period. The reaction mixture was stirred for 30 min then 2-ethyl-2-thiopseudourea (1.3 g, 6.7 mmol) in methanol (2.5 mL) was added at once. The mixture was heated and maintained at reflux for 2 h, cooled to room temperature and acidified to pH 6 with concentrated HCl. The resulting slurry was kept in ice bath for 30 minutes. The solid was collected and was rinsed with methanol. The solid was dried under vacuum to give 154 mg of the title compound. Mass spectrum 171.1 (CI, M+1).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US06498165B1 |
| Quelldatensatz | uspto-grants-2002_12 |
| ORD ID | ord-c01007e9015e4fbebc490d43cfe309be |
| Quellennotiz | uspto-grants-2002_12 |