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Acrylic Acid → Acryloxythexyldiisopropylsilane

HRID 2301009
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HRID 2301009 반응식
[C:1]([OH:5])(=[O:4])[CH:2]=[CH2:3].C(C1C=C(C)C=C(C(C)(C)C)C=1O)(C)(C)C.C(N(CC)CC)C.[C:29]([Si:35]([CH:40]([CH3:42])[CH3:41])([CH:37]([CH3:39])[CH3:38])Cl)([CH:32]([CH3:34])[CH3:33])([CH3:31])[CH3:30]>C1(C)C=CC=CC=1>[C:1]([O:5][Si:35]([C:29]([CH:32]([CH3:34])[CH3:33])([CH3:31])[CH3:30])([CH:40]([CH3:41])[CH3:42])[CH:37]([CH3:38])[CH3:39])(=[O:4])[CH:2]=[CH2:3]
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참가 물질

6

반응물 4

HCID 6581Acrylic AcidHCID 8471TriethylamineHCID 314042,6-Di-tert-butyl-4-methylphenolHCID 9899472Thexyldiisopropylchlorosilane

생성물 1

HCID 12040554Acryloxythexyldiisopropylsilane

시약·촉매·용매 1

HCID 1140Toluene용매

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온도
80 °C

실험 절차

A flask equipped with a stirrer, reflux condenser, dropping funnel and thermometer was charged with 14.4 g (0.2 mol) of acrylic acid, 120 ml of toluene, and 0.06 g of 2,6-di-tert-butyl-4-methylphenol. At room temperature, 22.3 g (0.22 mol) of triethylamine was added dropwise over one hour. At the end of dropwise addition, the flask was heated at 80° C. After the internal temperature became constant, 47.0 g (0.20 mol) of thexyldiisopropylchlorosilane was added dropwise over two hours. After the completion of dropwise addition, the reaction solution was stirred for 5 hours at 80° C. The reaction solution was then cooled to room temperature, and the resulting hydrochloric acid salt removed by filtration. The filtrate was distilled, collecting 38.6 g of a fraction having a boiling point of 87-92° C./0.13 kPa.

후처리

  1. customA flask equipped with a stirrer
  2. temperaturereflux condenser
  3. additionAt the end of dropwise addition
  4. additionAfter the completion of dropwise addition
  5. temperatureThe reaction solution was then cooled to room temperature
  6. customthe resulting hydrochloric acid salt removed by filtration
  7. distillationThe filtrate was distilled
  8. customcollecting 38.6 g of a fraction

출처 및 근거

ORD 기록
ord-37823d561bbf4f5f91e59e27c21aafc9
출처 데이터셋
uspto-grants-2002_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06498264B2

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