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Hydrochloric Acid → 2-Fluoro-4-[2-(4-propylphenyl)ethynyl]phenyl acetylene

HRID 850238
ノート
印刷プレビュー

反応式

HRID 850238 の反応式
[F:1][C:2]1[CH:7]=[C:6]([C:8]#[C:9][C:10]2[CH:15]=[CH:14][C:13]([CH2:16][CH2:17][CH3:18])=[CH:12][CH:11]=2)[CH:5]=[CH:4][C:3]=1[C:19]#[C:20][Si](C)(C)C.[OH-].[K+].Cl>C(O)C.O>[F:1][C:2]1[CH:7]=[C:6]([C:8]#[C:9][C:10]2[CH:11]=[CH:12][C:13]([CH2:16][CH2:17][CH3:18])=[CH:14][CH:15]=2)[CH:5]=[CH:4][C:3]=1[C:19]#[CH:20]
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 313Hydrochloric AcidHCID 14797Potassium HydroxideHCID 19362374HCID 19362374、化合物

生成物 1

HCID 541902552-Fluoro-4-[2-(4-propylphenyl)ethynyl]phenyl acetylene収率 98.8%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 962Water溶媒

実験手順

22 mmol of 1-[2-fluoro-4-[2-(4-propylphenyl)-ethynyl]phenyl]-2-trimethylsilylacetylene and 10 g of potassium hydroxide were dissolved in 100 ml of ethanol and 10 ml of water, and the solution was stirred at 40° C. for 6 hours. After completion of the agitation, the reaction solution was poured into dilute hydrochloric acid and extracted with toluene. The organic layer was washed with water, dried over anhydrous magnesium sulfate and concentrated under reduced pressure to afford a brown oily product. This product was isolated and purified by a silica gel column chromatography to afford 5.7 g of 2-fluoro-4-[2-(4-propylphenyl)ethynyl]phenyl acetylene as a colourless solid.

後処理

  1. extractionextracted with toluene
  2. washThe organic layer was washed with water
  3. dry with materialdried over anhydrous magnesium sulfate
  4. concentrationconcentrated under reduced pressure
  5. customto afford a brown oily product
  6. customThis product was isolated
  7. custompurified by a silica gel column chromatography

出典と根拠

ORDレコード
ord-d0fed464de92498abc6c0adac68762f7
出典データセット
uspto-grants-2000_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06017467

反応ノート

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