HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Hydrochloric Acid → Thiophene-2,5-dicarboxylic acid di-1,3-benzodioxol-5-ylmethyl ester
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Hydrochloric Acid | HCID 313 | — |
| Edukt | Dichloromethane | HCID 6344 | — |
| Edukt | Cesium carbonate | HCID 10796 | — |
| Edukt | 2,5-Thiophenedicarboxylic acid | HCID 20273 | — |
| Edukt | 1,3-Benzodioxole, 5-(chloromethyl)- | HCID 88713 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Lösungsmittel | Dimethylformamide | HCID 6228 | — |
| Produkt | Thiophene-2,5-dicarboxylic acid di-1,3-benzodioxol-5-ylmethyl ester | HCID 69693184 | — |
Reaktionsschritte
Cesium carbonate (4.7 g, 14.4 mmol) was added to a stirred solution of 2,5-thiophenedicarboxylic acid in dimethylformamide (35 mL) under an inert atmosphere at room temperature. After 5 minutes, a solution of 3,4-methylenedioxybenzyl chloride in dichloromethane (3.7 mL, 14.3 mmol) was added. After 24 hours the mixture was stirred into water (150 mL) and acidified with dilute aqueous HCl. After several hours, the precipitate was filtered off, rinsed with water, and dried to afford 0.6 g of thiophene-2,5-dicarboxylic acid di-1,3-benzodioxol-5-ylmethyl ester. Recrystallization of a sample from ethanol gave product with a mp 141-148° C.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US06924276B2 |
| Quelldatensatz | uspto-grants-2005_08 |
| ORD ID | ord-e262d475e39c4c9497b1e3db39202161 |
| Quellennotiz | uspto-grants-2005_08 |