Reaktion #343297
ord-18928221ff0b43fb8386a7c651984276
Reaktionsgleichung
Reagenzien
Keine
Lösungsmittel
Reaktionsbedingungen
Detaillierte Bedingungen
See reaction.notes.procedure_details.
Aufarbeitung
- 1Sonstigethe ice bath is removed
- 2workup.ADDITIONTHF (5 mL) is added
- 3Temperaturthe mixture heated
- 4Temperaturat reflux for two hours
- 5workup.WAITset aside overnight
- 6FiltrationThe cooled mixture is filtered
- 7Waschenthe collected solid washed with ether
Vorschrift
2-Amino-2,3-dimethylbutyramide (0.71 g) all in one portion is added to a stirred solution of 3-chlorothieno[3,2-b]pyridine-5,6-dicarboxylic acid anhydride, (1.2 g) in THF (1.0 mL). After standing for five minutes, the ice bath is removed and the reaction stirred at room temperature for 28 hours. THF (5 mL) is added and the mixture heated at reflux for two hours and then set aside overnight. The cooled mixture is filtered and the collected solid washed with ether to give 1.4 g of the desired 5-[(1-carbamoyl-1,2-dimethylpropyl)carbamoyl]3-chlorothieno[3,2-b]pyridine-6-carboxylic acid.