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Vinylidene fluoride → (1-Fluorovinyl)dimethylphenylsilane

HRID 400623
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HRID 400623 반응식
[Li].[CH3:2][Si:3]([CH3:11])([C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1)Cl.[SiH3][Li].[F:14][C:15](F)=[CH2:16]>C1COCC1>[F:14][C:15]([Si:3]([CH3:11])([CH3:2])[C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1)=[CH2:16]
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참가 물질

6

반응물 4

HCID 6369Vinylidene fluoride3회HCID 13029ChlorodimethylphenylsilaneHCID 3028194LithiumHCID 178506968HCID 178506968, 화합물

생성물 1

HCID 60026366(1-Fluorovinyl)dimethylphenylsilane

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To a suspension of 4.4 g of lithium wire cut into small pieces in 200 mL of anhydrous THF stirred under argon and cooled on ice (internal temperature <10° C.) was added dimethylphenyl-chlorosilane in 5 mL portions over 1 hour. The deep red color of the silyl lithium reagent appeared after approximately 0.75 hour. The mixture was stirred on ice for an additional 5 hours (internal temperature remained between 5° C. and 10° C.). The mixture was cooled on a dry ice/acetone bath and 1,1-difluoroethylene was introduced by filling a balloon connected to the reaction mixture and the reagent cylinder using a three-way valve. The balloon was filled with 1,1-difluoroethylene and emptied into the reaction mixture 10 times. The mixture was allowed to warm to room temperature (effervescence observed, probably from unreacted 1,1-difluoroethylene). The mixture was diluted with 200 mL of hexanes and filtered through a cotton wool plug. The filtrate was washed with water, dried, filtered, and concentrated in vacuo. Four fractional distillations under vacuum through a Vigreux column gave 4.6 g of product.

후처리

  1. temperaturecooled on ice (internal temperature <10° C.)
  2. stirringThe mixture was stirred on ice for an additional 5 hours (internal temperature remained between 5° C. and 10° C.)
  3. temperatureThe mixture was cooled on a dry ice/acetone bath
  4. filtrationfiltered through a cotton wool plug
  5. washThe filtrate was washed with water
  6. customdried
  7. filtrationfiltered
  8. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-22e73bbb78f740d786a181cd35b9046a
출처 데이터셋
uspto-grants-2014_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08741897B2

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