Potassium Carbonate → HCID 86685014, Verbindung

HRID 719046

Reaktionsgleichung

[CH3:1][C:2]1([CH3:22])[C:14]2[C:6]([N:7]=[C:8]3[C:13]=2[CH:12]=[CH:11][CH:10]=[CH:9]3)=[CH:5][C:4]2[CH:15]=[C:16]3[C:21]([C:3]1=2)=[CH:20][CH2:19][CH:18]=[CH:17]3.I[C:24]1[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1.S(=O)(O)[O-].[Na+].C(C1C=C(C(C)(C)C)C=C(C(O)=O)C=1O)(C)(C)C.C(=O)([O-])[O-].[K+].[K+]>[Cu].C(C1C=CC=CC=1)CCCCCCCCCCC>[CH3:1][C:2]1([CH3:22])[C:14]2[C:6]([N:7]=[C:8]3[C:13]=2[CH:12]=[CH:11][CH:10]=[CH:9]3)=[CH:5][C:4]2[CH:15]=[C:16]3[C:21]([C:3]1=2)=[CH:20][CH:19]([C:24]1[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1)[CH:18]=[CH:17]3

Komponenten

Reaktionsbedingungen

Temperatur: 170 °C

Versuchsvorschrift

The resulting 12,12-dimethyl-10,12-dihydroindeno[2,1-b]carbazole (7.8 g), iodobenzene (3.7 ml), sodium bisulfite (0.43 g), a copper powder (0.17 g), 3,5-di(tert-butyl)salicylic acid (0.69 g), potassium carbonate (5.71 g), and dodecylbenzene (10 ml) were added to a nitrogen-substituted reaction vessel, heated, and stirred at 170° C. for 10 hours. The mixture was cooled to 100° C., extracted by adding toluene (100 ml), concentrated under reduced pressure, and crystallized using n-hexane (30 ml) to obtain a pale yellow powder of 12,12-dimethyl-10-phenyl-10,12-dihydroindeno[2,1-b]carbazole (8.73 g; yield 88.3%).

Aufarbeitung

temperatureheated
temperatureThe mixture was cooled to 100° C.
extractionextracted
additionby adding toluene (100 ml)
concentrationconcentrated under reduced pressure
customcrystallized

Quellen und Nachweise

ORD-Eintrag: ord-e750f15685eb4227a37c2a101453df7e
Quelldatensatz: uspto-grants-2015_11
DOI: 10.6084/m9.figshare.5104873.v1
Patentnummer: US09196837B2

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