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Toluene → 4-(9,9-Dioctyl-7-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-YL)-9H-fluoren-2-YL)-N,N-diphenylaniline

HRID 11189
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HRID 11189 반응식
Br[C:2]1[CH:20]=[CH:19][C:5]([N:6]([C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)[C:7]2[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=2)=[CH:4][CH:3]=1.[CH2:21]([C:29]1([CH2:60][CH2:61][CH2:62][CH2:63][CH2:64][CH2:65][CH2:66][CH3:67])[C:41]2[CH:40]=[C:39]([B:42]3[O:46][C:45]([CH3:48])([CH3:47])[C:44]([CH3:50])([CH3:49])[O:43]3)[CH:38]=[CH:37][C:36]=2[C:35]2[C:30]1=[CH:31][C:32](B1OC(C)(C)C(C)(C)O1)=[CH:33][CH:34]=2)[CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH3:28].C(=O)([O-])[O-].[Na+].[Na+].C1(C)C=CC=CC=1>CCCCCCCC[N+](CCCCCCCC)(CCCCCCCC)C.[Cl-].CC(C)=O.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.[Pd].C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C1(C)C=CC=CC=1.CCCCCC.O>[CH2:60]([C:29]1([CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH3:28])[C:30]2[CH:31]=[C:32]([C:2]3[CH:20]=[CH:19][C:5]([N:6]([C:13]4[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=4)[C:7]4[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=4)=[CH:4][CH:3]=3)[CH:33]=[CH:34][C:35]=2[C:36]2[C:41]1=[CH:40][C:39]([B:42]1[O:43][C:44]([CH3:49])([CH3:50])[C:45]([CH3:47])([CH3:48])[O:46]1)=[CH:38][CH:37]=2)[CH2:61][CH2:62][CH2:63][CH2:64][CH2:65][CH2:66][CH3:67]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

11

반응물 4

HCID 1140TolueneHCID 10340Sodium CarbonateHCID 6428384-BromotriphenylamineHCID 219820749,9-Dioctylfluorene-2,7-diboronic acid bis(pinacol) ester

생성물 1

HCID 219820994-(9,9-Dioctyl-7-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-YL)-9H-fluoren-2-YL)-N,N-diphenylaniline

시약·촉매·용매 6

HCID 21218
Trioctylmethylammonium chloride
촉매
HCID 15220664Palladium--triphenylphosphane (1/1)촉매
HCID 178418397HCID 178418397, 화합물촉매
HCID 180Acetone용매
HCID 962Water용매
HCID 21889329Toluene hexane용매

실험 절차

4-Bromo-N,N-diphenylaniline (19.44 g, 60 mmole, 1 equiv), 2-[9,9-dioctyl-7-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)-9H-fluoren-2-yl]-4,4,5,5-tetramethyl-1,3,2-dioxaborolane (76.9 g, 120 mmole, 2 equiv), Aliquat™ 336 (tricaprylylmethylammonium chloride) (6 g, 15 mmole, 0.25 equiv) and 2M sodium carbonate solution (75 mL, 150 mmole, 2.5 equiv) were added to 600 mL of toluene. This was purged with a stream of nitrogen for about 30 min. Under a nitrogen purge, tetrakis(triphenylphosphine palladium (0) (348 mg, 0.30 mmole, 0.005 equiv) was added. The reaction mixture was then refluxed for 16 hrs. The reaction was cooled to room temperature and water added. The organic layer was separated and washed with water followed by brine. Drying of the organic layer over Na2SO4 and evaporation of the solvent gave a light yellow solid. This was suspended in acetone and the mixture brought to reflux and then allowed to stand at room temperature overnight. Filtration of the solid and concentration of the filtrate gave a solid that was subjected to column chromatography (toluene:hexane 3:7) to give 4-[9,9-dioctyl-7-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)-9H-fluoren-2-yl]-N,N-diphenylaniline.

후처리

  1. customThis was purged with a stream of nitrogen for about 30 min
  2. customUnder a nitrogen purge
  3. temperatureThe reaction mixture was then refluxed for 16 hrs
  4. customThe organic layer was separated
  5. washwashed with water
  6. dry with materialDrying of the organic layer over Na2SO4 and evaporation of the solvent
  7. customgave a light yellow solid
  8. temperatureto reflux
  9. filtrationFiltration of the solid and concentration of the filtrate
  10. customgave a solid

출처 및 근거

ORD 기록
ord-b2dbec03729041cdb275660146cddfe5
출처 데이터셋
uspto-grants-2006_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07094902B2

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