Potassium Carbonate → HCID 86685014、化合物

HRID 719046

反応式

HRID 719046 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.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

参加物

8

反応物 5

HCID 11430Potassium CarbonateHCID 11575IodobenzeneHCID 882083,5-Bis(1,1-dimethylethyl)-2-hydroxybenzoic acidHCID 23665763Sodium BisulfiteHCID 8668501212,12-Dimethyl-10,12-dihydroindeno[2,1-b]carbazole

生成物 1

HCID 86685014HCID 86685014、化合物収率 88.3%

試薬・触媒・溶媒 2

HCID 23978Copper触媒HCID 31237Dodecylbenzene溶媒

反応条件

温度
170 °C

実験手順

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%).

後処理

  1. temperatureheated
  2. temperatureThe mixture was cooled to 100° C.
  3. extractionextracted
  4. additionby adding toluene (100 ml)
  5. concentrationconcentrated under reduced pressure
  6. customcrystallized

出典と根拠

ORDレコード
ord-e750f15685eb4227a37c2a101453df7e
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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