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Methacrylic Acid → Methacryloxythexyldiisopropylsilane

HRID 2301008
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HRID 2301008 반응식
[C:1]([OH:6])(=[O:5])[C:2]([CH3:4])=[CH2:3].C(C1C=C(C)C=C(C(C)(C)C)C=1O)(C)(C)C.C(N(CC)CC)C.[C:30]([Si:36]([CH:41]([CH3:43])[CH3:42])([CH:38]([CH3:40])[CH3:39])Cl)([CH:33]([CH3:35])[CH3:34])([CH3:32])[CH3:31]>C1(C)C=CC=CC=1>[C:1]([O:6][Si:36]([C:30]([CH:33]([CH3:35])[CH3:34])([CH3:32])[CH3:31])([CH:41]([CH3:42])[CH3:43])[CH:38]([CH3:39])[CH3:40])(=[O:5])[C:2]([CH3:4])=[CH2:3]
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참가 물질

6

반응물 4

HCID 4093Methacrylic AcidHCID 8471TriethylamineHCID 314042,6-Di-tert-butyl-4-methylphenolHCID 9899472Thexyldiisopropylchlorosilane

생성물 1

HCID 12040553Methacryloxythexyldiisopropylsilane

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 17.2 g (0.2 mol) of methacrylic 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 43.2 g of a fraction having a boiling point of 92-97° 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 43.2 g of a fraction

출처 및 근거

ORD 기록
ord-a6ce985694a246aa91e6318bba65f23d
출처 데이터셋
uspto-grants-2002_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06498264B2

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