ホームMCPワークベンチSkills
ホームワークベンチ通知マイページ
llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
  1. ホーム
  2. /反応

Sodium Carbonate → HCID 58160694、化合物

HRID 1943514
ノート
印刷プレビュー

反応式

HRID 1943514 の反応式
Br[C:2]1[S:3][CH:4]=[CH:5][CH:6]=1.[CH2:7]([C:10]1[CH:15]=[CH:14][C:13]([C:16]2[CH:21]=[CH:20][C:19](B(O)O)=[C:18]([F:25])[CH:17]=2)=[CH:12][CH:11]=1)[CH2:8][CH3:9].C(=O)([O-])[O-].[Na+].[Na+]>C1(C)C=CC=CC=1.C(O)C.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>[CH2:7]([C:10]1[CH:15]=[CH:14][C:13]([C:16]2[CH:21]=[CH:20][C:19]([C:2]3[S:3][CH:4]=[CH:5][CH:6]=3)=[C:18]([F:25])[CH:17]=2)=[CH:12][CH:11]=1)[CH2:8][CH3:9]
参加物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 138512-BromothiopheneHCID 53402576B-(3-Fluoro-4'-propyl(1,1'-biphenyl)-4-yl)boronic acid

生成物 1

HCID 58160694HCID 58160694、化合物

試薬・触媒・溶媒 2

HCID 178418397HCID 178418397、化合物触媒HCID 21863594
Toluene ethanol
溶媒

実験手順

A mixture of 25.3 g (0.16 mol) of 2-bromothiophene, 40.0 g (0.16 mol) of 4′-propyl-3-fluoro-4-biphenylboronic acid, 8.5 g (7.4 mmol) of tetrakis(triphenylphosphine)palladium(0) and 170 ml of 2 N sodium carbonate solution in 420 ml of toluene/ethanol (1:2) is refluxed for 18 h. After cooling, the organic phase is separated off, and the aqueous phase is extracted a number of times with toluene. The combined organic phases are washed with water and sat. sodium chloride solution. The solution is dried using sodium sulfate and evaporated to dryness. The residue is purified by column chromatography (SiO2, n-heptane:toluene=9:1). The further purification is carried out by recrystallisation from ethanol and n-heptane, giving 2-(4′-propyl-3-fluorobiphenyl-4-yl)thiophene as a colourless solid (m.p. 88° C.).

後処理

  1. temperatureis refluxed for 18 h
  2. temperatureAfter cooling
  3. customthe organic phase is separated off
  4. extractionthe aqueous phase is extracted a number of times with toluene
  5. washThe combined organic phases are washed with water and sat. sodium chloride solution
  6. customThe solution is dried
  7. customevaporated to dryness
  8. customThe residue is purified by column chromatography (SiO2, n-heptane:toluene=9:1)
  9. customThe further purification
  10. customis carried out by recrystallisation from ethanol and n-heptane

出典と根拠

ORDレコード
ord-b4374e14821b4f45b42b5d0526e9b7ca
出典データセット
uspto-grants-2013_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08394293B2

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート