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Methyl Methanesulfonate → HCID 86654377, 화합물

HRID 537707
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HRID 537707 반응식
[CH3:1][O:2][Si:3]([CH2:8][CH2:9][C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][N:11]=1)([O:6][CH3:7])[O:4][CH3:5].[CH3:16][S:17]([O:20]C)(=[O:19])=[O:18]>C(OCC)(=O)C>[CH3:16][S:17]([O-:20])(=[O:19])=[O:18].[CH3:1][O:2][Si:3]([CH2:8][CH2:9][C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][N+:11]=1[CH3:16])([O:6][CH3:7])[O:4][CH3:5]
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참가 물질

4

반응물 2

HCID 4156Methyl MethanesulfonateHCID 27605062-(Trimethoxysilylethyl)pyridine

생성물 1

HCID 86654377HCID 86654377, 화합물

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매2회

실험 절차

5.0 g of 2-(trimethoxysilylethyl)pyridine and 18 g of ethyl acetate were charged into a 100 mL flask to be dissolved. While stirring the resultant mixed solution with a magnetic stirrer, to the mixed solution, a solution in which 3.6 g of methyl methanesulfonate was dissolved in 24 g of ethyl acetate was gradually added at room temperature in a nitrogen atmosphere. The reaction mixture was refluxed over 3 days and therefrom, ethyl acetate was distilled off under reduced pressure. The resultant concentrate was dropped into 100 mL of diethyl ether and therefrom, 2-(trimethoxysilylethyl)pyridine and methyl methanesulfonate as by-products were removed. This purification was repeated three times and then remaining diethyl ether was distilled off under reduced pressure, followed by dissolving the resultant concentrate in methanol to obtain a 30% methanol solution of trimethoxysilylethylmethylpyridinium methanesulfonate.

후처리

  1. dissolutionto be dissolved
  2. additionmixed solution with a magnetic stirrer
  3. additionwas gradually added at room temperature in a nitrogen atmosphere
  4. temperatureThe reaction mixture was refluxed over 3 days
  5. distillationethyl acetate was distilled off under reduced pressure
  6. concentrationThe resultant concentrate
  7. additionwas dropped into 100 mL of diethyl ether
  8. custom2-(trimethoxysilylethyl)pyridine and methyl methanesulfonate as by-products were removed
  9. customThis purification
  10. distillationremaining diethyl ether was distilled off under reduced pressure
  11. dissolutionby dissolving the resultant
  12. concentrationconcentrate in methanol

출처 및 근거

ORD 기록
ord-9aa9d2637d92437493cf34c8c67db34c
출처 데이터셋
uspto-grants-2014_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08864894B2

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