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Sodium Carbonate → 5-Bromo-2-(4-octylphenyl)pyridine

HRID 2227114
ノート
印刷プレビュー

反応式

HRID 2227114 の反応式
[Br:1][C:2]1[C:3](Br)=[N:4][CH:5]=[CH:6][CH:7]=1.[CH2:9]([C:17]1[CH:22]=[CH:21][C:20](B(O)O)=[CH:19][CH:18]=1)[CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH3:16].C(=O)([O-])[O-].[Na+].[Na+]>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.C1(C)C=CC=CC=1>[Br:1][C:2]1[CH:7]=[CH:6][C:5]([C:20]2[CH:19]=[CH:18][C:17]([CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH3:16])=[CH:22][CH:21]=2)=[N:4][CH:3]=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

6

反応物 3

HCID 10340Sodium CarbonateHCID 8171022,3-DibromopyridineHCID 4197992(4-octylphenyl)boronic Acid

生成物 1

HCID 184718205-Bromo-2-(4-octylphenyl)pyridine収率 95%

試薬・触媒・溶媒 2

HCID 178418397HCID 178418397、化合物触媒
HCID 1140
Toluene
溶媒

反応条件

温度
100 °C

実験手順

To a 1000 mL round bottom flask equipped with a stirbar was added dibromopyridine 7C (22.506 g), boronic acid 7B (22.356 g), tetrakis(triphenylphosphine)palladium(0) (3.294 g), saturated sodium carbonate solution (238 mL), and toluene (190 mL). A reflux condenser was attached and the reaction was heated at 100° C. for 24 hours. The cooled reaction mixture was extracted with 1:1 hexane:ethyl acetate, and the combined organic layers were washed with brine and dried over magnesium sulfate and the solvent was removed in vacuo. The solid product was dissolved in dichloromethane, placed on silica gel, and silica gel filtered. The elution solvents were hexane, which removed a higher Rf side product, and 2.5% E/H, resulting in 31.251 g of solid. The product was recrystallized from acetonitrile to give 30.125 g of a white solid.

後処理

  1. customTo a 1000 mL round bottom flask equipped with a stirbar
  2. customA reflux condenser was attached
  3. customThe cooled reaction mixture
  4. extractionwas extracted with 1:1 hexane
  5. washethyl acetate, and the combined organic layers were washed with brine
  6. dry with materialdried over magnesium sulfate
  7. customthe solvent was removed in vacuo
  8. dissolutionThe solid product was dissolved in dichloromethane
  9. filtrationfiltered
  10. customremoved a higher Rf side product, and 2.5% E/H

出典と根拠

ORDレコード
ord-084f9497f27543ada529675940335893
出典データセット
uspto-grants-2002_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06413448B1

反応ノート

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