HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Hydrochloric Acid → 5-Methyl-4-oxo-2-(thiophen-3-ylmethyl)-3,4-dihydrothieno[2,3-d]pyrimidine-6-carboxylic acid
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Hydrochloric Acid | HCID 313 | — |
| Edukt | Sodium Hydroxide | HCID 14798 | — |
| Edukt | Ethyl 5-methyl-4-oxo-2-(thiophen-3-ylmethyl)-3,4-dihydrothieno[2,3-d]pyrimidine-6-carboxylate | HCID 68664667 | — |
| Lösungsmittel | Ethanol | HCID 702 | — |
| Produkt | 5-Methyl-4-oxo-2-(thiophen-3-ylmethyl)-3,4-dihydrothieno[2,3-d]pyrimidine-6-carboxylic acid | HCID 16091083 | 92,2% |
Reaktionsschritte
A mixture of 379 mg of ethyl 5-methyl-4-oxo-2-(thiophen-3-ylmethyl)-3,4-dihydrothieno[2,3-d]pyrimidine-6-carboxylate as synthesized in Production Example 1, 3.4 mL of 1N aqueous sodium hydroxide solution and 2.2 mL of ethanol was heated under reflux for 2 hours. After cooling off, the reaction liquid was poured on ice, rendered acidic with diluted hydrochloric acid, and the precipitated crystals were recovered by filtration. After washing with water, the crystals were dried by heating under reduced pressure, to provide 320 mg of 5-methyl-4-oxo-2-(thiophen-3-ylmethyl)-3,4-dihydrothieno[2,3-d]pyrimidine-6-carboxylic acid.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08377944B2 |
| Quelldatensatz | uspto-grants-2013_02 |
| ORD ID | ord-bdef864c039d47bc9d99340187e10c79 |
| Quellennotiz | uspto-grants-2013_02 |