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

HRID 2275919
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HRID 2275919 반응식
[CH3:1][C:2]1([CH3:28])[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][C:17]([C:22]1[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=1)=[CH:16][CH:15]=4.[H-].[Na+].Cl[C:32]1[N:37]=[C:36]([C:38]2[CH:43]=[CH:42][CH:41]=[CH:40][CH:39]=2)[N:35]=[C:34]([C:44]2[CH:49]=[CH:48][CH:47]=[CH:46][CH:45]=2)[N:33]=1>CN(C)C=O>[C:44]1([C:34]2[N:35]=[C:36]([C:38]3[CH:39]=[CH:40][CH:41]=[CH:42][CH:43]=3)[N:37]=[C:32]([N:13]3[C:12]4[CH:11]=[C:10]5[C:2]([CH3:28])([CH3:1])[C:3]6[C:8]([C:9]5=[CH:21][C:20]=4[C:19]4[C:14]3=[CH:15][CH:16]=[C:17]([C:22]3[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=3)[CH:18]=4)=[CH:7][CH:6]=[CH:5][CH:4]=6)[N:33]=2)[CH:49]=[CH:48][CH:47]=[CH:46][CH:45]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 196982-Chloro-4,6-diphenyl-1,3,5-triazineHCID 24758Sodium hydrideHCID 6679746212,12-Dimethyl-7-phenyl-10,12-dihydro-10-azaindeno[2,1-b]fluorene

생성물 1

HCID 6679759610-(4,6-Diphenyl-1,3,5-triazin-2-yl)-12,12-dimethyl-7-phenyl-10,12-dihydro-10-azaindeno[2,1-b]fluorene

시약·촉매·용매 1

HCID 6228Dimethylformamide
용매
2회

실험 절차

10 g (27.7 mmol) of 12,12-dimethyl-7-phenyl-10,12-dihydro-10-azaindeno-[2,1-b]fluorene are dissolved in 275 ml of dimethylformamide under a protective-gas atmosphere, and 1.45 g of NaH, 60% in mineral oil (36 mmol), are added. After 1 h at room temperature, a solution of 2-chloro-4,6-diphenyl-1,3,5-triazine (8.2 g, 30.5 mmol) in 75 ml of dimethylformamide is added dropwise. The reaction mixture is then 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 14.7 g (24.9 mmol, 90%).

후처리

  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

출처 및 근거

ORD 기록
ord-48697e7d96a14110af314f3d1d8dea3e
출처 데이터셋
uspto-grants-2015_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09126970B2

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