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2-Fluorobenzoyl chloride → 11-(2-Ethylhexyl)-8-(2-fluorobenzoyl)-11H-benzo[a]carbazole-5-yl-(2,4,6-trimethylphenyl)-methanone

HRID 2203245
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HRID 2203245 반응식
[CH2:1]([CH:3]([CH2:22][CH2:23][CH2:24][CH3:25])[CH2:4][N:5]1[C:17]2[C:12](=[CH:13][CH:14]=[C:15]3[CH:21]=[CH:20][CH:19]=[CH:18][C:16]3=2)[C:11]2[C:6]1=[CH:7][CH:8]=[CH:9][CH:10]=2)[CH3:2].[CH3:26][C:27]1[CH:35]=[C:34]([CH3:36])[CH:33]=[C:32]([CH3:37])[C:28]=1[C:29](Cl)=[O:30].[Al+3].[Cl-].[Cl-].[Cl-].[F:42][C:43]1[CH:51]=[CH:50][CH:49]=[CH:48][C:44]=1[C:45](Cl)=[O:46]>C(Cl)Cl>[CH2:1]([CH:3]([CH2:22][CH2:23][CH2:24][CH3:25])[CH2:4][N:5]1[C:17]2[C:12](=[CH:13][C:14]([C:29]([C:28]3[C:27]([CH3:26])=[CH:35][C:34]([CH3:36])=[CH:33][C:32]=3[CH3:37])=[O:30])=[C:15]3[CH:21]=[CH:20][CH:19]=[CH:18][C:16]3=2)[C:11]2[C:6]1=[CH:7][CH:8]=[C:9]([C:45](=[O:46])[C:44]1[CH:48]=[CH:49][CH:50]=[CH:51][C:43]=1[F:42])[CH:10]=2)[CH3:2]
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참가 물질

6

반응물 4

HCID 98082-Fluorobenzoyl chlorideHCID 970382,4,6-Trimethylbenzoyl chlorideHCID 6451240Aluminum(III) Chloride2회HCID 6713010811-(2-Ethylhexyl)-11H-benzo[a]carbazole

생성물 1

HCID 6809414611-(2-Ethylhexyl)-8-(2-fluorobenzoyl)-11H-benzo[a]carbazole-5-yl-(2,4,6-trimethylphenyl)-methanone

시약·촉매·용매 1

HCID 6344
Dichloromethane
용매

실험 절차

To 11-(2-ethylhexyl)-11H-benzo[a]carbazole (47.16 g; 143.0 mmol) in CH2Cl2 (400 mL) are added 2,4,6-trimethylbenzoyl chloride (27.45 g; 150.0 mmol) and AlCl3 (20.00 g; 150.0 mmol) at 0° C. After stirring at room temperature for 2 hours, AlCl3 (22.93 g; 172.0 mmol) is added at 0° C. and 2-fluorobenzoyl chloride (23.78 g; 150.0 mmol) is added dropwise, and then the mixture is stirred at room temperature for 3 hours. The reaction mixture is poured into ice-water, and the crude product is extracted twice with CH2Cl2. The combined organic layer is washed with water and brine, dried over MgSO4. After 230 ml of n-hexane are added, the CH2Cl2 is removed by concentration to give a beige solid. It is collected by filtration, and washed with n-hexane. Then it is dried to give a beige solid (81.81 g; 95.7%). The structure is confirmed by 1H-NMR spectrum (CDCl3). δ [ppm]: 0.84 (t), 0.89 (t), 1.18-1.42 (m), 2.20 (s), 2.28-2.31 (m), 2.40 (s), 4.72-4.76 (m), 6.96 (s), 7.19 (t), 7.29 (t), 7.52-7.60 (m), 7.70-7.84 (m), 8.38 (s), 8.63-8.66 (m), 9.56 (d); 19F-NMR spectrum (CDCl3). δ [ppm]: −111.58.

후처리

  1. stirringthe mixture is stirred at room temperature for 3 hours
  2. extractionthe crude product is extracted twice with CH2Cl2
  3. washThe combined organic layer is washed with water and brine
  4. dry with materialdried over MgSO4
  5. additionAfter 230 ml of n-hexane are added
  6. customthe CH2Cl2 is removed by concentration
  7. customto give a beige solid
  8. filtrationIt is collected by filtration
  9. washwashed with n-hexane
  10. customThen it is dried
  11. customto give a beige solid (81.81 g; 95.7%)

출처 및 근거

ORD 기록
ord-de0cecd199dd45459afd352ad29f0965
출처 데이터셋
uspto-grants-2016_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09365515B2

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