Reaktion #2289627

ord-cd66312c138b46f2951aee25d0e2933e

Reaktionsbedingungen

Temperatur
60°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    FiltrationThe precipitated solid was filtered
  2. 2
    Sonstigedried

Vorschrift

9-Ethyl-6,6-dimethyl-8-(4-morpholin-4-yl-piperidin-1-yl)-11-oxo-6,11-dihydro-5H-benzo[b]carbazole-3-carbonitrile was dissolved in a mixture of 10 v/w of methyl ethyl ketone, 4 v/w of water, and 3 v/w of acetic acid at 60° C. To the dissolved solution, 1 v/w of hydrochloric acid (2 N) was added dropwise. After stirring at 60° C. for 30 minutes, 25 v/w of ethanol was added dropwise. The precipitated solid was filtered and dried to give 9-ethyl-6,6-dimethyl-8-(4-morpholin-4-yl-piperidin-1-yl)-11-oxo-6,11-dihydro-5H-benzo[b]carbazole-3-carbonitrile monohydrochloride salt. 9-Ethyl-6,6-dimethyl-8-(4-morpholin-4-yl-piperidin-1-yl)-11-oxo-6,11-dihydro-5H-benzo[b]carbazole-3-carbonitrile monohydrochloride salt obtained was pulverized by using a jet mill.

Quelle

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