Dichloromethane → HCID 66834116, Verbindung

HRID 2275080Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2275080
ClCCl.[CH3:4][C:5]1([CH3:38])[C:17]2[NH:16][C:15]3[C:10](=[CH:11][CH:12]=[C:13]([C:18]#[N:19])[CH:14]=3)[C:9]=2[C:8](=[O:20])[C:7]2[CH:21]=[CH:22][C:23]([O:25][CH:26]3[CH2:31][O:30]C(C4C=CC=CC=4)[O:28][CH2:27]3)=[CH:24][C:6]1=2>O>[OH:30][CH2:31][CH:26]([CH2:27][OH:28])[O:25][C:23]1[CH:22]=[CH:21][C:7]2[C:8](=[O:20])[C:9]3[C:10]4[C:15](=[CH:14][C:13]([C:18]#[N:19])=[CH:12][CH:11]=4)[NH:16][C:17]=3[C:5]([CH3:4])([CH3:38])[C:6]=2[CH:24]=1

Komponenten

4

Edukt 2

HCID 6344DichloromethaneHCID 668341506,6-Dimethyl-11-oxo-8-(2-phenyl-[1,3]dioxan-5-yloxy)-6,11-dihydro-5H-benzo[b]carbazole-3-carbonitrile

Produkt 1

HCID 66834116HCID 66834116, VerbindungAusbeute 66,4 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

Anhydrous ferric trichloride (56 mg, 5 eq.) was added to the dichloromethane (2 mL) suspension of 6,6-dimethyl-11-oxo-8-(2-phenyl-[1,3]dioxan-5-yloxy)-6,11-dihydro-5H-benzo[b]carbazole-3-carbonitrile (Compound A7-13-1, 13 mg, 0.028 mmol), and stirred at room temperature for 1 hr. The reaction solution was added to water, and then extracted with ethyl acetate. The organic layer was washed with saturated brine and dried over sodium sulfate. The drying agent was removed by filtration and the residues obtained after concentration under reduced pressure were purified by high performance liquid chromatography to obtain the title compound (7 mg, 46%).

Aufarbeitung

  1. extractionextracted with ethyl acetate
  2. washThe organic layer was washed with saturated brine
  3. dry with materialdried over sodium sulfate
  4. customThe drying agent was removed by filtration
  5. customthe residues obtained
  6. concentrationafter concentration under reduced pressure
  7. customwere purified by high performance liquid chromatography

Quellen und Nachweise

ORD-Eintrag
ord-c73aaab9fb584f32a6e4fdc6eebb171f
Quelldatensatz
uspto-grants-2015_09
Patentnummer
US09126931B2

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