Ethanol → Diethoxy(methyl)(3-(oxiran-2-ylmethoxy)propyl)silane

HRID 1276703노트

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HRID 1276703 반응식
[CH3:1][SiH:2]([O:6][CH2:7][CH3:8])[O:3][CH2:4][CH3:5].C(O)C.[CH2:12]([O:16][CH2:17][CH:18]=[CH2:19])[CH:13]1[O:15][CH2:14]1>C(O)(=O)C>[CH2:12]([O:16][CH2:17][CH2:18][CH2:19][Si:2]([CH3:1])([O:6][CH2:7][CH3:8])[O:3][CH2:4][CH3:5])[CH:13]1[O:15][CH2:14]1

참가 물질

5

반응물 3

HCID 702EthanolHCID 7838Allyl glycidyl etherHCID 74848Methyldiethoxysilane

생성물 1

HCID 62467Diethoxy(methyl)(3-(oxiran-2-ylmethoxy)propyl)silane수율 82%

시약·촉매·용매 1

HCID 176Acetic Acid용매

반응 조건

온도
85 °C

실험 절차

Again, to the apparatus of Example 3 were pressure charged 49.6 lb [22.5 kg] (168.2 mol) of methyldiethoxysilane from a 10 gallon Pope can. After addition of the 20.0 g of CPA ethanol solution (15 ppm Pt) and 21.0 ml (460 ppm) of acetic acid through the handhole, the reactor was kept under nitrogen purge, sealed and heated to 85° C. Allyl glycidyl ether (50.6 lb [23 kg], 20 mole % excess or 210.8 mol) was added through a line to the mixture in the reactor from a pressurized can. The AGE was added at a rate that kept the reaction temperature between 85 and 95° C. After two hours, the addition was complete and the hydrosilation lites were stripped. The crude product was vacuum distilled at 104-121° C. (3-7 mm Hg) to yield 75.5 pounds (31.23 kg) of γ-glycidoxypropylmethyldiethoxysilane with an average purity of 99.0%. This represents a conversion of 82.3%. Again present were the silane scrambled products γ-glycidoxy-propyldimethyl(ethoxy) silane (0.39% by GC) and γ-glycidoxypropyltriethoxysilane (0.27% by GC).

후처리

  1. custompurge
  2. customsealed
  3. additionThe AGE was added at a rate that
  4. customthe reaction temperature between 85 and 95° C
  5. additionthe addition
  6. distillationdistilled at 104-121° C. (3-7 mm Hg)

출처 및 근거

ORD 기록
ord-1c9bf5e554f543159f38d0f56e126f30
출처 데이터셋
uspto-grants-2000_12
특허 번호
US06166238

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