Reaktion #2289622

ord-bec1aa780c734eb79da87779a66b2e35

Reaktionsgleichung

CC1(C)c2cc(N3CCN(C4COC4)CC3)c(Br)cc2C(=O)c2c1[nH]c1cc(C#N)ccc21
9-Bromo-6,6-dimethyl-8-(4-oxetan-3-yl-piperazin-1-yl)-11-oxo-6,11-dihydro-5H-benzo[b]carbazole-3-carbonitrile
Cl
hydrochloric acid
→
CC1(C)c2cc(N3CCN(C4COC4)CC3)c(Br)cc2C(=O)c2c1[nH]c1cc(C#N)ccc21.Cl
9-bromo-6,6-dimethyl-8-(4-oxetan-3-yl-piperazin-1-yl)-11-oxo-6,11-dihydro-5H-benzo[b]carbazole-3-carbonitrile monohydrochloride salt

Edukte

CC1(C)c2cc(N3CCN(C4COC4)CC3)c(Br)cc2C(=O)c2c1[nH]c1cc(C#N)ccc21
9-Bromo-6,6-dimethyl-8-(4-oxetan-3-yl-piperazin-1-yl)-11-oxo-6,11-dihydro-5H-benzo[b]carbazole-3-carbonitrile
Cl
hydrochloric acid

Reagenzien

Keine

Lösungsmittel

CS(C)=O
DMSO

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.DISSOLUTIONdissolved
  2. 2
    SonstigeAfter freeze-drying
  3. 3
    Sonstigethe mixture was crystallized from ethanol containing 25% water

Vorschrift

9-Bromo-6,6-dimethyl-8-(4-oxetan-3-yl-piperazin-1-yl)-11-oxo-6,11-dihydro-5H-benzo[b]carbazole-3-carbonitrile was added with 1.05 eq. of 6 N hydrochloric acid and DMSO and dissolved therein. After freeze-drying, the mixture was crystallized from ethanol containing 25% water to give 9-bromo-6,6-dimethyl-8-(4-oxetan-3-yl-piperazin-1-yl)-11-oxo-6,11-dihydro-5H-benzo[b]carbazole-3-carbonitrile monohydrochloride salt.

Quelle

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