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Sodium Carbonate → 2-[3-(9,10-Diphenyl-2-anthryl)phenyl]dibenzofuran

HRID 719044
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HRID 719044 반응식
Br[C:2]1[CH:3]=[C:4]([C:8]2[CH:21]=[CH:20][C:19]3[C:10](=[C:11]([C:28]4[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=4)[C:12]4[C:17]([C:18]=3[C:22]3[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=3)=[CH:16][CH:15]=[CH:14][CH:13]=4)[CH:9]=2)[CH:5]=[CH:6][CH:7]=1.[CH:34]1[C:42]2[C:41]3[CH:43]=[CH:44][CH:45]=[CH:46][C:40]=3[O:39][C:38]=2[CH:37]=[CH:36][C:35]=1B(O)O.C1(C)C=CC=CC=1P(C1C=CC=CC=1C)C1C=CC=CC=1C.C(=O)([O-])[O-].[Na+].[Na+]>C([O-])(=O)C.[Pd+2].C([O-])(=O)C.C1(C)C=CC=CC=1.CCCCCC.C(O)C>[C:28]1([C:11]2[C:12]3[C:17]([C:18]([C:22]4[CH:23]=[CH:24][CH:25]=[CH:26][CH:27]=4)=[C:19]4[C:10]=2[CH:9]=[C:8]([C:4]2[CH:5]=[C:6]([C:35]5[CH:36]=[CH:37][C:38]6[O:39][C:40]7[CH:46]=[CH:45][CH:44]=[CH:43][C:41]=7[C:42]=6[CH:34]=5)[CH:7]=[CH:2][CH:3]=2)[CH:21]=[CH:20]4)=[CH:16][CH:15]=[CH:14][CH:13]=3)[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

9

반응물 4

HCID 10340Sodium CarbonateHCID 80271Tri-o-tolylphosphineHCID 12032376Dibenzo(b,d)furan-2-ylboronic Acid (contains varying amounts of Anhydride)HCID 575364512-(3-Bromophenyl)-9,10-diphenylanthracene

생성물 1

HCID 582618792-[3-(9,10-Diphenyl-2-anthryl)phenyl]dibenzofuran수율 29.1%

시약·촉매·용매 4

HCID 167845palladium(II) acetate촉매HCID 702Ethanol용매HCID 1140Toluene용매2회HCID 8058Hexane용매

실험 절차

In a 50 mL three-neck flask were put 1.2 g (2.4 mmol) of 2-(3-bromophenyl)-9,10-diphenylanthracene, 0.52 g (2.4 mmol) of dibenzofuran-2-boronic acid, and 0.18 g (0.60 mmol) of tri(ortho-tolyl)phosphine. The air in the flask was replaced with nitrogen. To this mixture were added 10 mL of toluene, 3.0 mL of ethanol, and 3.0 mL of an aqueous solution of sodium carbonate (2.0 mol/L). While the pressure was reduced, this mixture was stirred to be degassed. To this mixture was added 27 mg (0.12 mmol) of palladium(II) acetate, and the mixture was stirred at 80° C. for 3 hours. Then, the aqueous layer of the obtained mixture was extracted with toluene, and the toluene solution and the organic layer were combined and washed with saturated brine. The organic layer was dried with magnesium sulfate. Then, this mixture was gravity filtered. The resulting filtrate was concentrated, and the obtained oily substance was purified by silica gel column chromatography to give a yellow oily substance. The chromatography was carried out using a mixed solvent having a 5:1 ratio of hexane to toluene as a developing solvent, whereby an oily substance was obtained. Recrystallization of the oily substance from a mixed solvent of toluene and hexane gave 0.40 g of a yellow powder in 29% yield, which was the substance to be produced.

후처리

  1. customIn a 50 mL three-neck flask were put
  2. customto be degassed
  3. stirringthe mixture was stirred at 80° C. for 3 hours
  4. extractionThen, the aqueous layer of the obtained mixture was extracted with toluene
  5. washwashed with saturated brine
  6. dry with materialThe organic layer was dried with magnesium sulfate
  7. filtrationfiltered
  8. concentrationThe resulting filtrate was concentrated
  9. customthe obtained oily substance was purified by silica gel column chromatography
  10. customto give a yellow oily substance
  11. customwas obtained
  12. customRecrystallization of the oily substance from a mixed solvent of toluene and hexane

출처 및 근거

ORD 기록
ord-1533aad2830e43b6ac0917260db3e9fb
출처 데이터셋
uspto-grants-2015_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09196836B2

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