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Oxalic Acid → Propylene glycol methyl ether acetate

HRID 252879
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HRID 252879 반응식
[O:1]1[CH:7]2[CH:2]1CC(CC[Si](OC)(OC)OC)[CH2:5][CH2:6]2.COC([SiH3])(OC)OC.C1([Si](OC)(OC)OC)C=CC=CC=1.[C:38](O)(=O)[C:39]([OH:41])=[O:40]>CO.O>[C:39]([O:41][CH:6]([CH3:5])[CH2:7][O:1][CH3:2])(=[O:40])[CH3:38]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 971Oxalic AcidHCID 18137TrimethoxyphenylsilaneHCID 18819EpoxycyclohexylethyltrimethoxysilaneHCID 101924291Trimethoxymethyl silane

생성물 1

HCID 7946Propylene glycol methyl ether acetate수율 100%

시약·촉매·용매 2

HCID 887Methanol용매
2회
HCID 962Water용매

반응 조건

온도
40 °C

실험 절차

In a 1000 ml glass flask, to a mixture of 150 g of methanol, 22 g of 2-(3,4-epoxycyclohexyl) ethyl trimethoxy silane, 77 g of trimethoxymethyl silane, 14 g of phenyl trimethoxy silane, and 1.5 g of oxalic acid was added dropwise a mixed solution of 40 g of deionized water and 20 g of methanol at a liquid temperature of 40 degrees C. After that, this solution was stirred for 12 hours at 40 degrees C. After the reaction finished, the solvent was removed under a reduced pressure. Thus-obtained residue was dissolved in 1000 ml of ethyl acetate, and washed with deionized water for washing. After the water layer was separated, the organic layer was washed twice with deionized water. To this organic layer was added 600 g of propylene glycol monomethyl ether acetate (PGMEA), and the contents were heated up to a liquid temperature of 40 degrees C. under a reduced pressure to remove ethyl acetate and to give a PGMEA solution of a polymer.

후처리

  1. customthe solvent was removed under a reduced pressure
  2. dissolutionThus-obtained residue was dissolved in 1000 ml of ethyl acetate
  3. washwashed with deionized water
  4. washfor washing
  5. customAfter the water layer was separated
  6. washthe organic layer was washed twice with deionized water
  7. additionTo this organic layer was added 600 g of propylene glycol monomethyl ether acetate (PGMEA)
  8. temperaturethe contents were heated up to a liquid temperature of 40 degrees C
  9. customunder a reduced pressure to remove ethyl acetate

출처 및 근거

ORD 기록
ord-edda5971751b461a9969fe51bbc46dfe
출처 데이터셋
uspto-grants-2011_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07868407B2

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