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Toluene → 7-(9H-Carbazol-3-yl)-12,12-dimethyl-10-phenyl-10,12-dihydro-10-azaindeno[2,1-b]fluorene

HRID 634554
ノート
印刷プレビュー

反応式

HRID 634554 の反応式
Br[C:2]1[CH:3]=[CH:4][C:5]2[NH:6][C:7]3[C:12]([C:13]=2[CH:14]=1)=[CH:11][CH:10]=[CH:9][CH:8]=3.B([C:18]1[CH:19]=[C:20]2[C:28](=[CH:29][CH:30]=1)[N:27]([C:31]1[CH:36]=[CH:35][CH:34]=[CH:33][CH:32]=1)[C:26]1[CH:25]=[C:24]3[C:37]([CH3:45])([CH3:44])[C:38]4[C:43]([C:23]3=[CH:22][C:21]2=1)=[CH:42][CH:41]=[CH:40][CH:39]=4)(O)O.C(=O)([O-])[O-].[Na+].[Na+].C1(C)C=CC=CC=1>O1CCOCC1.C1C=CC([P]([Pd]([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1.O>[CH:4]1[C:5]2[NH:6][C:7]3[C:12](=[CH:11][CH:10]=[CH:9][CH:8]=3)[C:13]=2[CH:14]=[C:2]([C:18]2[CH:19]=[C:20]3[C:28](=[CH:29][CH:30]=2)[N:27]([C:31]2[CH:36]=[CH:35][CH:34]=[CH:33][CH:32]=2)[C:26]2[CH:25]=[C:24]4[C:37]([CH3:45])([CH3:44])[C:38]5[C:43]([C:23]4=[CH:22][C:21]3=2)=[CH:42][CH:41]=[CH:40][CH:39]=5)[CH:3]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 4

HCID 1140TolueneHCID 10340Sodium CarbonateHCID 2524463-BromocarbazoleHCID 866960867-Borono12,12-dimethyl-10-phenyl-10,12-dihydro-10-aza-indeno[2,1-b]fluorene

生成物 1

HCID 676095847-(9H-Carbazol-3-yl)-12,12-dimethyl-10-phenyl-10,12-dihydro-10-azaindeno[2,1-b]fluorene

試薬・触媒・溶媒 3

HCID 178418397
HCID 178418397、化合物
触媒
HCID 962Water溶媒
HCID 312751,4-Dioxane溶媒

実験手順

14.07 g (57.18 mmol) of 3-bromo-9H-carbazole 22, 25.37 g (62.90 mmol) of compound 13 and 6.75 g of sodium carbonate are suspended in 1800 ml of dioxane, 1800 ml of toluene and 750 ml of water. 3.38 g (2.93 mmol) of Pd(PPh3)4 are added to this suspension. The reaction mixture is heated under reflux for 5 h. After cooling, the precipitated solid is filtered off with suction, washed with water and ethanol and dried. The residue is extracted with hot toluene and recrystallised from toluene. The yield is 19.5 g (65%).

後処理

  1. temperatureThe reaction mixture is heated
  2. temperatureunder reflux for 5 h
  3. temperatureAfter cooling
  4. filtrationthe precipitated solid is filtered off with suction
  5. washwashed with water and ethanol
  6. customdried
  7. extractionThe residue is extracted with hot toluene
  8. customrecrystallised from toluene

出典と根拠

ORDレコード
ord-54890b748f6c4946847fbc3580f2afd7
出典データセット
uspto-grants-2016_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09324954B2

反応ノート

読み込み中…

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