Potassium Carbonate → HCID 86685020、化合物

HRID 719055

反応式

HRID 719055 の反応式
[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.Br[C:24]1[CH:36]=[CH:35][C:34]2[C:33]3[C:28](=[CH:29][CH:30]=[CH:31][CH:32]=3)[C:27]([CH3:38])([CH3:37])[C:26]=2[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+].C(C1C=CC=CC=1)CCCCCCCCCCC>[Cu]>[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:36]=[CH:35][C:34]2[C:33]4[C:28](=[CH:29][CH:30]=[CH:31][CH:32]=4)[C:27]([CH3:38])([CH3:37])[C:26]=2[CH:25]=1)[CH:18]=[CH:17]3

参加物

8

反応物 6

HCID 11430Potassium CarbonateHCID 31237DodecylbenzeneHCID 882083,5-Bis(1,1-dimethylethyl)-2-hydroxybenzoic acidHCID 109456062-Bromo-9,9-dimethylfluoreneHCID 23665763Sodium BisulfiteHCID 8668501212,12-Dimethyl-10,12-dihydroindeno[2,1-b]carbazole

生成物 1

HCID 86685020HCID 86685020、化合物収率 80.2%

試薬・触媒・溶媒 1

HCID 23978Copper触媒

反応条件

温度
180 °C

実験手順

12,12-Dimethyl-10,12-dihydroindeno[2,1-b]carbazole synthesized in Example 1 (5.5 g), 2-bromo-9,9-dimethyl-9H-fluorene (6.4 g), sodium bisulfite (0.3 g), a copper powder (0.1 g), 3,5-di(tert-butyl)salicylic acid (0.5 g), potassium carbonate (4.0 g), and dodecylbenzene (5 ml) were added to a nitrogen-substituted reaction vessel, heated, and stirred at 180° C. for 29 hours. The mixture was cooled to 100° C., and insoluble matter was removed by filtration after adding toluene (80 ml), and a filtrate was concentrated. Crystallization using n-hexane (20 ml) was performed to obtain an ocher powder of 12,12-dimethyl-10-(9,9-dimethyl-9H-fluorene-2-yl)-10,12-dihydroindeno[2,1-b]carbazole (7.4 g; yield 80.0%)

後処理

  1. temperatureheated
  2. temperatureThe mixture was cooled to 100° C.
  3. custominsoluble matter was removed by filtration
  4. additionafter adding toluene (80 ml)
  5. concentrationa filtrate was concentrated
  6. customCrystallization

出典と根拠

ORDレコード
ord-dd83ce3cc8cf4d9e9e690d815fd0a03a
出典データセット
uspto-grants-2015_11
特許番号
US09196837B2

関連ノート

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