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

HRID 2121318

Reaktionsgleichung

Reaktionsgleichung von HRID 2121318
[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

Komponenten

6

Edukt 3

HCID 176Acetic AcidHCID 887MethanolHCID 865871472-ethyl-2-adamantyl Methacrylate p-acetoxystyrene

Produkt 1

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

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 142844-(Dimethylamino)pyridineKatalysatorHCID 962WaterLösungsmittel

Versuchsvorschrift

A flask was charged with 250 g of the 2-ethyl-2-adamantyl methacrylate/p-acetoxystyrene (20:80) copolymer obtained in Reference Example 3, 10.3 g (0,084 mol) of 4-dimethylaminopyridine and 202 g of methanol, and the mixture was kept for 20 hours with stirring under reflux. After cooling, the reaction solution was neutralized with 7.6 g (0.126 mol) of glacial-acetic acid, followed by pouring into a large amount of water to obtain a precipitate. The polymer (the precipitate) thus obtained was filtered and then dissolved into acetone. An operation of pouring the solution into a large amount of water was repeated for three times to obtain a precipitate and purify the same. Amount of the obtained copolymer of 2-ethyl-2-adamantyl methacrylate and p-hydroxystyrene was 95.9 g. Also, the polymer has a weight average molecular weight of about 8,600 and a degree of dispersion of 1.65, and a copolymerization ratio thereof was determined to be about 20:80 using a nuclear magnetic resonance (13C-NMR) spectrometer. This resin will be referred to as “resin B1”.

Aufarbeitung

  1. temperatureunder reflux
  2. temperatureAfter cooling
  3. customto obtain a precipitate
  4. customThe polymer (the precipitate) thus obtained
  5. filtrationwas filtered
  6. dissolutiondissolved into acetone
  7. additionAn operation of pouring the solution into a large amount of water
  8. customto obtain a precipitate
  9. custompurify the same

Quellen und Nachweise

ORD-Eintrag
ord-a350ecb65fc64f08990d215c59aa86f2
Quelldatensatz
uspto-grants-2004_02
Patentnummer
US06696218B2

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