Acetic Acid → 2-ethyl-2-adamantyl Methacrylate p-hydroxystyrene

HRID 2306526

반응식

HRID 2306526 반응식
[C:1]([O:6][C:7]1([CH2:17][CH3:18])[CH:14]2[CH2:15][CH:10]3[CH2:11][CH:12]([CH2:16][CH:8]1[CH2:9]3)[CH2:13]2)(=[O:5])[C:2]([CH3:4])=[CH2:3].C([O:22][C:23]1[CH:30]=[CH:29][C:26]([CH:27]=[CH2:28])=[CH:25][CH:24]=1)(=O)C.CO.C(O)(=O)C>CN(C)C1C=CN=CC=1.O>[C:1]([O:6][C:7]1([CH2:17][CH3:18])[CH:8]2[CH2:16][CH:12]3[CH2:11][CH:10]([CH2:15][CH:14]1[CH2:13]3)[CH2:9]2)(=[O:5])[C:2]([CH3:4])=[CH2:3].[OH:22][C:23]1[CH:30]=[CH:29][C:26]([CH:27]=[CH2:28])=[CH:25][CH:24]=1

참가 물질

7

반응물 4

HCID 176Acetic AcidHCID 887MethanolHCID 758214-Ethenylphenyl acetateHCID 98136452-Ethyl-2-methacryloyloxyadamantane

생성물 1

HCID 225083922-ethyl-2-adamantyl Methacrylate p-hydroxystyrene

시약·촉매·용매 2

HCID 142844-(Dimethylamino)pyridine촉매HCID 962Water용매

실험 절차

Into a flask were charged 250 g of the copolymer of 2-ethyl-2-adamantyl methacrylate and p-acetoxystyrene (20:80) obtained in Synthesis Example 4, 10.4 g (0.084 mol) of 4-dimethylaminopyridine and 202 g of methanol, and aged for 20 hours under reflux. After cooling, the reaction liquid was neutralized with 7.6 g (0.126 mol) of glacial acetic acid and poured into a large amount of water to precipitate a polymer. The deposited polymer was filtrated, dissolved in acetone, then, poured into a large amount of water to cause precipitation, and this operation was repeated three times in total for purification.

후처리

  1. temperatureunder reflux
  2. temperatureAfter cooling
  3. customthe reaction liquid
  4. customto precipitate a polymer
  5. filtrationThe deposited polymer was filtrated
  6. dissolutiondissolved in acetone
  7. additionpoured into a large amount of water
  8. customprecipitation
  9. customtotal for purification

출처 및 근거

ORD 기록
ord-2db065eb04064f0e83e45ff1399c260f
출처 데이터셋
uspto-grants-2004_12
특허 번호
US06828079B2

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