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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Dimethyl Sulfoxide → 3[o-(2-Propenyl)phenoxy]propyl trimethoxysilane

HRID 236628
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HRID 236628 반응식
[CH2:1]([C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=1[OH:10])[CH:2]=[CH2:3].[OH-].[Na+].CS(C)=O.Cl[CH2:18][CH2:19][CH2:20][Si:21]([O:26][CH3:27])([O:24][CH3:25])[O:22][CH3:23]>C1(C)C=CC=CC=1>[CH2:1]([C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=1[O:10][CH2:18][CH2:19][CH2:20][Si:21]([O:26][CH3:27])([O:24][CH3:25])[O:22][CH3:23])[CH:2]=[CH2:3]
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참가 물질

6

반응물 4

HCID 679Dimethyl SulfoxideHCID 14798Sodium HydroxideHCID 156242-AllylphenolHCID 624493-(Trimethoxysilyl)propyl chloride

생성물 1

HCID 138791743[o-(2-Propenyl)phenoxy]propyl trimethoxysilane수율 90%

시약·촉매·용매 1

HCID 1140Toluene용매

반응 조건

온도
115 °C

실험 절차

Using the general procedure described in Example 1 a reactor was charged with 73.7 g (0.55 mole) of o-allylphenol, 43.28 g of a 50% by weight aqueous solution of sodium hydroxide (0.54 mole NaOH), 112 cc dimethylsulfoxide and 120 cc toluene. The resultant mixture was heated to the boiling point for six hours under a nitrogen atmosphere to remove all of the water present by azeotropic distillation. The reaction mixture was then allowdd to cool to about 75° C., at which time 109 g (0.56 mole) of 3-chloropropyl trimethoxysilane was added dropwise while the reaction mixture was stirred. Following completion of the addition the reaction mixture was heated at 115° C. for about 16 hours, following which the mixture was allowed to cool and was filtered to remove any solid material. The solvents were then removed under a pressure of about 15 mm of mercury at a temperature of about 60° C. The pressure was then reduced to 2 mm of mercury and the material boiling at 146° C. was collected. The weight of this fraction was equivalent to a yield of 90% based on starting materials. Analysis by vapor phase chromatography indicated that the purity of the product was greater than 98%. The infrared and nuclear magnetic resonance spectra of the product were consistent with the proposed structure.

후처리

  1. customto remove all of the water present
  2. distillationby azeotropic distillation
  3. additionwas added dropwise while the reaction mixture
  4. additioncompletion of the addition the reaction mixture
  5. temperatureto cool
  6. filtrationwas filtered
  7. customto remove any solid material
  8. customThe solvents were then removed under a pressure of about 15 mm of mercury at a temperature of about 60° C
  9. customthe material boiling at 146° C. was collected

출처 및 근거

ORD 기록
ord-bf768ea7638c4a38b9f5f70d99d80c70
출처 데이터셋
uspto-grants-1987_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04645844

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