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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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1H,1H,2H,2H-Perfluorooctyldimethylchlorosilane → HCID 86663263, 화합물

HRID 1408492
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HRID 1408492 반응식
[F:1][C:2]([F:25])([C:9]([F:24])([F:23])[C:10]([F:22])([F:21])[C:11]([F:20])([F:19])[C:12]([F:18])([F:17])[C:13]([F:16])([F:15])[F:14])[CH2:3][CH2:4][Si:5]([CH3:8])([CH3:7])Cl.[C:26]([Mg]Br)#[CH:27]>C1COCC1>[F:1][C:2]([F:25])([C:9]([F:24])([F:23])[C:10]([F:22])([F:21])[C:11]([F:20])([F:19])[C:12]([F:18])([F:17])[C:13]([F:16])([F:15])[F:14])[CH2:3][CH2:4][Si:5]([C:26]#[CH:27])([CH3:8])[CH3:7]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 1453821H,1H,2H,2H-PerfluorooctyldimethylchlorosilaneHCID 178418486HCID 178418486, 화합물

생성물 1

HCID 86663263HCID 86663263, 화합물수율 96%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

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온도
60 °C

실험 절차

In an oven-dried 250-mL round bottom flask, 3,3,4,4,5,5,6,6,7,7,8,8,8-tridecafluorooctyldimethylchlorosilane (9.67 g, 21.9 mmol) was dissolved in 20 mL anhydrous THF. Ethynylmagnesium bromide (50 mL, 25 mmol, 0.5 M in THF) was added and the mixture was heated to 60° C. for 12 hr. After allowing the mixture to cool to room temperature, the reaction was quenched by the dropwise addition of water, followed by the addition of dilute sulfuric acid to dissolve the magnesium salts. The organic layer was separated, washed with water (3×20 mL) and brine, dried over magnesium sulfate, filtered and concentrated under vacuum. The crude product was purified by chromatography on silica gel using hexane as an eluant. Removal of solvent yielded 9.0 g (21 mmol, 96%) of the product as a colorless liquid. Analysis of the colorless product provided the following data: 1H-NMR (200 MHz, CDCl3) δ=2.4 (s, 1H), 2.1 (m, 2H), 0.8 (m, 2H), 0.2 (s, 6H).

후처리

  1. temperatureto cool to room temperature
  2. customthe reaction was quenched by the dropwise addition of water
  3. additionfollowed by the addition of dilute sulfuric acid
  4. dissolutionto dissolve the magnesium salts
  5. customThe organic layer was separated
  6. washwashed with water (3×20 mL) and brine
  7. dry with materialdried over magnesium sulfate
  8. filtrationfiltered
  9. concentrationconcentrated under vacuum
  10. customThe crude product was purified by chromatography on silica gel
  11. customRemoval of solvent

출처 및 근거

ORD 기록
ord-84dc760a22074a3cb7c86cf1c2fbcbc4
출처 데이터셋
uspto-grants-2014_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08920679B2

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