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Ethanol → Propylene glycol methyl ether acetate

HRID 252877
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HRID 252877 반응식
[CH2:1]([OH:3])[CH3:2].[OH-].C([N+](CC)(CC)CC)C.[O:14]1[CH:20]2[CH:15]1CC(CC[Si](OC)(OC)OC)[CH2:18][CH2:19]2.C1([Si](OC)(OC)[O:37]C)C=CC=CC=1>C(OCC)(=O)C.O>[C:1]([O:37][CH:19]([CH3:18])[CH2:20][O:14][CH3:15])(=[O:3])[CH3:2]
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참가 물질

7

반응물 4

HCID 702EthanolHCID 6509Tetraethylammonium HydroxideHCID 18137TrimethoxyphenylsilaneHCID 18819Epoxycyclohexylethyltrimethoxysilane

생성물 1

HCID 7946Propylene glycol methyl ether acetate수율 100%

시약·촉매·용매 2

HCID 962Water용매
HCID 8857
Ethyl Acetate
용매

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온도
40 °C

실험 절차

In a 3000 ml glass flask, 1400 g of ethanol, 700 g of pure water, and 50 g of 25% tetraethylammonium hydroxide were placed, and stirred. To this mixture was added dropwise a mixture of 139 g of 2-(3,4-epoxycyclohexyl) ethyl trimethoxy silane and 32 g of phenyl trimethoxy silane at a liquid temperature of 40 degrees C. After that, the solution was stirred for 2 hours at 40 degrees C. After the reaction finished, the reaction was quenched by adding 35 g of acetic acid, and ethanol was removed under a reduced pressure. To thus-obtained solution was added 2000 ml of ethyl acetate, and a water layer was separated. An organic layer was washed twice with ultrapure water. To this contents 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. additionTo this mixture was added dropwise
  2. stirringAfter that, the solution was stirred for 2 hours at 40 degrees C
  3. customthe reaction was quenched
  4. additionby adding 35 g of acetic acid, and ethanol
  5. customwas removed under a reduced pressure
  6. customTo thus-obtained solution
  7. customa water layer was separated
  8. washAn organic layer was washed twice with ultrapure water
  9. additionTo this contents was added 600 g of propylene glycol monomethyl ether acetate (PGMEA)
  10. customunder a reduced pressure to remove ethyl acetate

출처 및 근거

ORD 기록
ord-801cd54d384742d9b5fc16aa6b1c4d54
출처 데이터셋
uspto-grants-2011_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07868407B2

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