Ethanol → Propylene glycol methyl ether acetate

HRID 252877

反応式

HRID 252877 の反応式
[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]

参加物

7

反応条件

温度
40 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-801cd54d384742d9b5fc16aa6b1c4d54
出典データセット
uspto-grants-2011_01
特許番号
US07868407B2

関連ノート

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