반응 #343297

ord-18928221ff0b43fb8386a7c651984276

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타the ice bath is removed
  2. 2
    workup.ADDITIONTHF (5 mL) is added
  3. 3
    온도the mixture heated
  4. 4
    온도at reflux for two hours
  5. 5
    workup.WAITset aside overnight
  6. 6
    여과The cooled mixture is filtered
  7. 7
    세척the collected solid washed with ether

실험 절차

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.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US04701208uspto-grants-1987_10