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2-Chloro-4,6-diphenyl-1,3,5-triazine → 7-Dibenzofuran-4-yl-10-(4,6-diphenyl-1,3,5-triazin-2-yl)-12,12-dimethyl-10,12-dihydro-10-azaindeno[2,1-b]fluorene

HRID 2275951
ノート
印刷プレビュー

反応式

HRID 2275951 の反応式
[CH:1]1[C:9]2[C:8]3[CH:10]=[CH:11][CH:12]=[CH:13][C:7]=3[O:6][C:5]=2[C:4]([C:14]2[CH:15]=[C:16]3[C:24](=[CH:25][CH:26]=2)[NH:23][C:22]2[CH:21]=[C:20]4[C:27]([CH3:35])([CH3:34])[C:28]5[C:33]([C:19]4=[CH:18][C:17]3=2)=[CH:32][CH:31]=[CH:30][CH:29]=5)=[CH:3][CH:2]=1.[H-].[Na+].Cl[C:39]1[N:44]=[C:43]([C:45]2[CH:50]=[CH:49][CH:48]=[CH:47][CH:46]=2)[N:42]=[C:41]([C:51]2[CH:56]=[CH:55][CH:54]=[CH:53][CH:52]=2)[N:40]=1>CN(C)C=O>[CH:1]1[C:9]2[C:8]3[CH:10]=[CH:11][CH:12]=[CH:13][C:7]=3[O:6][C:5]=2[C:4]([C:14]2[CH:15]=[C:16]3[C:24](=[CH:25][CH:26]=2)[N:23]([C:39]2[N:44]=[C:43]([C:45]4[CH:50]=[CH:49][CH:48]=[CH:47][CH:46]=4)[N:42]=[C:41]([C:51]4[CH:52]=[CH:53][CH:54]=[CH:55][CH:56]=4)[N:40]=2)[C:22]2[CH:21]=[C:20]4[C:27]([CH3:35])([CH3:34])[C:28]5[C:33]([C:19]4=[CH:18][C:17]3=2)=[CH:32][CH:31]=[CH:30][CH:29]=5)=[CH:3][CH:2]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 196982-Chloro-4,6-diphenyl-1,3,5-triazineHCID 24758Sodium hydrideHCID 667975987-Dibenzofuran-4-yl-12,12-dimethyl-10,12-dihydro-10-azaindeno[2,1-b]fluorene

生成物 1

HCID 667978447-Dibenzofuran-4-yl-10-(4,6-diphenyl-1,3,5-triazin-2-yl)-12,12-dimethyl-10,12-dihydro-10-azaindeno[2,1-b]fluorene

試薬・触媒・溶媒 1

HCID 6228
Dimethylformamide
溶媒
2 回

実験手順

16.6 g (58.78 mmol) of 7-dibenzofuran-4-yl-12,12-dimethyl-10,12-dihydro-10-azaindeno[2,1-b]fluorene are dissolved in 225 ml of dimethylformamide under a protective-gas atmosphere, and 2.8 g of 60% NaH in mineral oil (70 mmol) are added. After 1 h at room temperature, a solution of 2-chloro-4,6-diphenyl-1,3,5-triazine (18.6 g, 66.2 mmol) in 75 ml of dimethylformamide is added dropwise. The reaction mixture is stirred at room temperature for 12 h. After this time, the reaction mixture is poured onto ice and extracted three times with dichloromethane. The combined organic phases are dried over Na2SO4 and evaporated. The residue is extracted with hot toluene, recrystallised from dichloromethane/isopropanol and finally sublimed in a high vacuum, the purity is 99.9%. The yield is 18.3 g (27 mmol, 45.7%).

後処理

  1. additionare added
  2. additionAfter this time, the reaction mixture is poured onto ice
  3. extractionextracted three times with dichloromethane
  4. dry with materialThe combined organic phases are dried over Na2SO4
  5. customevaporated
  6. extractionThe residue is extracted with hot toluene
  7. customrecrystallised from dichloromethane/isopropanol

出典と根拠

ORDレコード
ord-100adca25c5549aea57c405d9bb73414
出典データセット
uspto-grants-2015_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09126970B2

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート