Reaktion #2289618

ord-1952870e6d774c6aa6359839fe36fe86

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeWith the same condition as the method for synthesizing the Compound
  2. 2
    FiltrationThe reaction solution was filtered
  3. 3
    Sonstigeto remove insoluble matters
  4. 4
    SonstigeThe residues obtained
  5. 5
    Einengenafter concentration under reduced pressure
  6. 6
    Sonstigewere purified by high performance liquid chromatography
  7. 7
    Sonstigeto obtain the Compound

Vorschrift

With the same condition as the method for synthesizing the Compound B3-32 (morpholine (6 μl, 1.5 eq.) and sodium triacetoxy borohydride (81 mg, 2.0 eq.) were added to THF (1 ml) solution of the Compound B2-29: 8-formyl-6,6-dimethyl-11-oxo-6,11-dihydro-5H-benzo[b]carbazole-3-carbonitrile (30 mg, 0.095 mmol), and stirred at room temperature for 1 hour. The reaction solution was filtered to remove insoluble matters. The residues obtained after concentration under reduced pressure were purified by high performance liquid chromatography to obtain the Compound B3-32 (6,6-dimethyl-8-morpholin-4-yl methyl-11-oxo-6,11-dihydro-5H-benzo carbazole-3-carbonitrile) (19 mg, 50%)), the title compound was synthesized from the Compound B3-13-2 and oxetan-3-one.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US09365514B2uspto-grants-2016_06