Reaktion #452260

ord-0269698e4f8849b7ad328d3b580ace77

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigethe ice bath is removed
  2. 2
    workup.ADDITIONTHF (5 mL) is added
  3. 3
    Temperaturthe mixture heated
  4. 4
    Temperaturat reflux for two hours
  5. 5
    workup.WAITset aside overnight
  6. 6
    FiltrationThe cooled mixture is filtered
  7. 7
    Waschenthe 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.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04608079uspto-grants-1986_08