Sodium hydride → 10-(4,6-Bis[1,1';3',1'']terphenyl-5'-yl-1,3,5-triazin-2-yl)-12,12-dimethyl-10,12-dihydro-10-azaindeno[2,1-b]fluorene

HRID 2275930ノート

反応式

HRID 2275930 の反応式
[CH3:1][C:2]1([CH3:22])[C:10]2=[CH:11][C:12]3[NH:13][C:14]4[C:19]([C:20]=3[CH:21]=[C:9]2[C:8]2[C:3]1=[CH:4][CH:5]=[CH:6][CH:7]=2)=[CH:18][CH:17]=[CH:16][CH:15]=4.[H-].[Na+].Cl[C:26]1[N:31]=[C:30]([C:32]2[CH:33]=[C:34]([C:44]3[CH:49]=[CH:48][CH:47]=[CH:46][CH:45]=3)[CH:35]=[C:36]([C:38]3[CH:43]=[CH:42][CH:41]=[CH:40][CH:39]=3)[CH:37]=2)[N:29]=[C:28]([C:50]2[CH:51]=[C:52]([C:62]3[CH:67]=[CH:66][CH:65]=[CH:64][CH:63]=3)[CH:53]=[C:54]([C:56]3[CH:61]=[CH:60][CH:59]=[CH:58][CH:57]=3)[CH:55]=2)[N:27]=1>CN(C)C=O>[C:62]1([C:52]2[CH:51]=[C:50]([C:28]3[N:29]=[C:30]([C:32]4[CH:37]=[C:36]([C:38]5[CH:39]=[CH:40][CH:41]=[CH:42][CH:43]=5)[CH:35]=[C:34]([C:44]5[CH:49]=[CH:48][CH:47]=[CH:46][CH:45]=5)[CH:33]=4)[N:31]=[C:26]([N:13]4[C:12]5[CH:11]=[C:10]6[C:2]([CH3:22])([CH3:1])[C:3]7[C:8]([C:9]6=[CH:21][C:20]=5[C:19]5[C:14]4=[CH:15][CH:16]=[CH:17][CH:18]=5)=[CH:7][CH:6]=[CH:5][CH:4]=7)[N:27]=3)[CH:55]=[C:54]([C:56]3[CH:57]=[CH:58][CH:59]=[CH:60][CH:61]=3)[CH:53]=2)[CH:63]=[CH:64][CH:65]=[CH:66][CH:67]=1

参加物

5

反応物 3

HCID 24758Sodium hydrideHCID 582991192,4-Di([1,1':3',1''-terphenyl]-5'-yl)-6-chloro-1,3,5-triazineHCID 665852047,7-Dimethyl-5,7-dihydroindeno[2,1-b]carbazole

生成物 1

HCID 6679787010-(4,6-Bis[1,1';3',1'']terphenyl-5'-yl-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 6228Dimethylformamide溶媒2 回

実験手順

11.3 g (40 mmol) of 12,12-dimethyl-10,12-dihydro-10-azaindeno[2,1-b]-fluorene are dissolved in 285 ml of dimethylformamide under a protective-gas atmosphere, and 1.9 g of 60% NaH in mineral oil (19 mmol) are added. After 1 h at room temperature, a solution of 2-chloro-4,6-bis-[1,1′;3′,1″]terphenyl-5′-yl-1,3,5-triazine (25.1 g, 44 mmol) in 315 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. The yield is 23 g (28 mmol, 70%).

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

出典と根拠

ORDレコード
ord-95855c69c19f42c99ebb511f4ab626fa
出典データセット
uspto-grants-2015_09
特許番号
US09126970B2

反応ノート

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