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Triethylamine → 2-(4-Bromophenyl)triphenylene

HRID 871813
ノート
印刷プレビュー

反応式

HRID 871813 の反応式
O1[CH:5]2[C:6]3[C:7]4[C:12]([C:13]5[C:18]([C:19]=3[CH:2]1[CH:3]=[CH:4]2)=[CH:17][CH:16]=[CH:15][CH:14]=5)=[CH:11][CH:10]=[CH:9][CH:8]=4.[Br:20][C:21]1[CH:26]=[CH:25][C:24](I)=[CH:23][CH:22]=1.BrC1C=CC=C(I)C=1.C(N(CC)CC)C>[Zn].Cl[Pd](Cl)([P](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1)[P](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1.C1(C)C=CC=CC=1>[Br:20][C:21]1[CH:26]=[CH:25][C:24]([C:15]2[CH:16]=[CH:17][C:18]3[C:19]4[C:6](=[CH:5][CH:4]=[CH:3][CH:2]=4)[C:7]4[C:12](=[CH:11][CH:10]=[CH:9][CH:8]=4)[C:13]=3[CH:14]=2)=[CH:23][CH:22]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

8

反応物 4

HCID 8471TriethylamineHCID 115221-Bromo-4-iodobenzeneHCID 11561Benzene, 1-bromo-3-iodo-HCID 126679791,4-Dihydro-1,4-epoxytriphenylene

生成物 1

HCID 581748542-(4-Bromophenyl)triphenylene収率 62%

試薬・触媒・溶媒 3

HCID 23994Zinc触媒
HCID 178418476
HCID 178418476、化合物
触媒
HCID 1140Toluene溶媒

反応条件

温度
110 °C

実験手順

Compound A (4.0 g, 16.4 mmol), zinc (10.72 g, 163.9 mmol), PdCl2(PPh3)2 (1.16 g, 1.7 mmol), and 1-bromo-4-iodobenzene (4.64 g, 16.4 mmol) or 1-bromo-3-iodobenzene were charged in a two-necked bottle. The bottle was then vacuumed and purged with nitrogen, and dried toluene (100 mL) and triethyl amine (23.0 mL, 165.9 mmol) were added to the bottle. The mixture in the bottle was heated to 110° C. for reaction for 24 hours, and the resulting was filtered to remove metal. The filtrate was condensed to remove the solvent, and then purified by chromatography with hexanes to obtain B (3.90 g, yield=62%) as white solid.

後処理

  1. additionwere added to the bottle
  2. filtrationthe resulting was filtered
  3. customto remove metal
  4. customcondensed
  5. customto remove the solvent
  6. custompurified by chromatography with hexanes
  7. customto obtain B (3.90 g, yield=62%) as white solid

出典と根拠

ORDレコード
ord-6174dcc545a14f29adf9fe3aa17eda30
出典データセット
uspto-grants-2015_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08974920B2

反応ノート

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