반응 #95670

ord-e33fddcbe4e3411bb8fa597335b0d2b0

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도the mixture is heated
  2. 2
    온도under reflux for 1 hour
  3. 3
    workup.WAITSubsequently, the mixture is left
  4. 4
    여과the separated crystals are filtered off
  5. 5
    세척washed with 2-propanol and water, there

실험 절차

100 ml of 2-propanol are treated with 100 mg of sodium hydride. 5 g of ethyl 8-fluoro-5,6-dihydro-5-methyl-6-oxo-4H-imidazo[1,5-a][1,4]benzodiazepine-3-carboxylate are added thereto and the mixture is heated to boiling under reflux for 1 hour. Subsequently, the mixture is left to cool to room temperature, the separated crystals are filtered off and washed with 2-propanol and water, there being obtained isopropyl 8-fluoro-5,6-dihydro-5-methyl-6-oxo-4H-imidazo[1,5-a][1,4]benzodiazepine-3-carboxylate of melting point 243°-244° C.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US04346032uspto-grants-1982_08