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

HRID 850238
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HRID 850238 반응식
[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]
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참가 물질

6

반응물 3

HCID 313Hydrochloric AcidHCID 14797Potassium HydroxideHCID 19362374HCID 19362374, 화합물

생성물 1

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

시약·촉매·용매 2

HCID 702Ethanol용매HCID 962Water용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-d0fed464de92498abc6c0adac68762f7
출처 데이터셋
uspto-grants-2000_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06017467

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