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Water → 1-[(E)-1,2-difluoro-2-(4-propylcyclohexyl)vinyl]-4-ethoxy-2,3-difluorobenzene

HRID 1841834
ノート
印刷プレビュー

反応式

HRID 1841834 の反応式
[F:1]/[C:2](/[CH:6]1[CH2:11][CH2:10][CH:9]([CH2:12][CH2:13][CH3:14])[CH2:8][CH2:7]1)=[C:3](/[F:5])\I.[F:15][C:16]1[C:21]([F:22])=[C:20]([O:23][CH2:24][CH3:25])[CH:19]=[CH:18][C:17]=1B(O)O.C(=O)([O-])[O-].[Na+].[Na+].O>C(O)C.C1(C)C=CC=CC=1>[F:5]/[C:3](/[C:17]1[CH:18]=[CH:19][C:20]([O:23][CH2:24][CH3:25])=[C:21]([F:22])[C:16]=1[F:15])=[C:2](/[F:1])\[CH:6]1[CH2:11][CH2:10][CH:9]([CH2:12][CH2:13][CH3:14])[CH2:8][CH2:7]1
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 4

HCID 962WaterHCID 10340Sodium CarbonateHCID 15135235B-(4-Ethoxy-2,3-difluorophenyl)boronic acidHCID 866743031-((Z)-1,2-difluoro-2-iodovinyl)-4-propylcyclohexane

生成物 1

HCID 673277251-[(E)-1,2-difluoro-2-(4-propylcyclohexyl)vinyl]-4-ethoxy-2,3-difluorobenzene

試薬・触媒・溶媒 1

HCID 21863594
Toluene ethanol
溶媒

実験手順

6.30 g (20.1 mmol) of 1-((Z)-1,2-difluoro-2-iodovinyl)-4-propylcyclohexane and 4.86 g (24.1 mmol) of 2,3-difluoro-4-ethoxybenzeneboronic acid are refluxed for 19 h together with 1.16 g (1.0 mmol) of tetrakistriphenylpalladium(0) and 20 ml (20 mmol) of sodium carbonate solution (2 M) in 90 ml of ethanol/toluene (2:1). Water is added, and the batch is extracted with MTBE. The aqueous phase is extracted with MTBE, and the combined organic phases are washed with water. The solution is dried using sodium sulfate and concentrated to dryness. The residue is purified by column chromatography (SiO2, n-heptane:1-chlorobutane=4:1). The further purification is carried out by recrystallisation from n-heptane, giving 1-[(E)-1,2-difluoro-2-(4-propylcyclohexyl)vinyl]-4-ethoxy-2,3-difluorobenzene as a colourless solid (m.p. 60° C.).

後処理

  1. extractionthe batch is extracted with MTBE
  2. extractionThe aqueous phase is extracted with MTBE
  3. washthe combined organic phases are washed with water
  4. customThe solution is dried
  5. concentrationconcentrated to dryness
  6. customThe residue is purified by column chromatography (SiO2, n-heptane:1-chlorobutane=4:1)
  7. customThe further purification
  8. customis carried out by recrystallisation from n-heptane

出典と根拠

ORDレコード
ord-e459ec64e4d5444990b74c50d79fdd09
出典データセット
uspto-grants-2015_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08945420B2

反応ノート

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