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Sodium Bicarbonate → HCID 58028448、化合物

HRID 1943520
ノート
印刷プレビュー

反応式

HRID 1943520 の反応式
[Na+].[CH2:2]([C:8]1[S:12][C:11](OB(O)[O-])=[CH:10][CH:9]=1)[CH2:3][CH2:4][CH2:5][CH2:6][CH3:7].Br[C:18]1[CH:23]=[CH:22][C:21]([C:24]2[CH:29]=[CH:28][C:27]([CH2:30][CH2:31][CH2:32][CH2:33][CH3:34])=[CH:26][CH:25]=2)=[C:20]([F:35])[CH:19]=1.C(=O)([O-])O.[Na+]>C1COCC1.O.CC(OC)(C)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>[F:35][C:20]1[CH:19]=[C:18]([C:11]2[S:12][C:8]([CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH3:7])=[CH:9][CH:10]=2)[CH:23]=[CH:22][C:21]=1[C:24]1[CH:29]=[CH:28][C:27]([CH2:30][CH2:31][CH2:32][CH2:33][CH3:34])=[CH:26][CH:25]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 3

HCID 516892Sodium BicarbonateHCID 227175154-Bromo-2-fluoro-4'-pentyl-1,1'-biphenylHCID 131730280HCID 131730280、化合物

生成物 1

HCID 58028448HCID 58028448、化合物

試薬・触媒・溶媒 3

HCID 178418397HCID 178418397、化合物触媒HCID 15413
tert-Butyl methyl ether
溶媒
HCID 21881883Oxolane--water (1/1)溶媒

実験手順

A mixture of 3.30 g (13.1 mmol) of 5-hexylthiophen-2-ylhydroxyboronic acid sodium salt, 4.20 g (13.1 mmol) of 4-bromo-2-fluoro-4′-pentylbiphenyl, 2.2 g (26.2 mmol) of sodium hydrogencarbonate and 0.70 g (0.61 mmol) of tetrakis(triphenylphosphine)palladium(0) in THF/water (1:1) is refluxed for 6 h. The mixture is diluted with MTBE, and the organic phase is separated off. The aqueous phase is extracted with MTBE. The combined organic phases are washed with sat. sodium chloride solution and dried using sodium sulfate. The solution is evaporated to dryness, and the residue is purified by column chromatography (SiO2, n-heptane). The further purification is carried out by recrystallisation from methanol/-pentane (5:1). 2-(2-Fluoro-4′-pentylbiphenyl-4-yl)-5-hexylthiophene is obtained as a colourless solid having an m.p. of 44° C.

後処理

  1. temperatureis refluxed for 6 h
  2. customthe organic phase is separated off
  3. extractionThe aqueous phase is extracted with MTBE
  4. washThe combined organic phases are washed with sat. sodium chloride solution
  5. customdried
  6. customThe solution is evaporated to dryness
  7. customthe residue is purified by column chromatography (SiO2, n-heptane)
  8. customThe further purification
  9. customis carried out by recrystallisation from methanol/-pentane (5:1)

出典と根拠

ORDレコード
ord-a745828eac674d2a92d6f02d31c3e488
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

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