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

HRID 2120034

反応式

HRID 2120034 の反応式
[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.C(O)(=O)C>CN(C)C1C=CN=CC=1.CO>[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

参加物

6

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 142844-(Dimethylamino)pyridine触媒HCID 887Methanol溶媒

実験手順

Into a flask were charged 250 g of the copolymer of 2-ethyl-2-adamantyl methacrylate and p-acetoxystyrene (30:70) obtained in Reference Example 7, 10.8 g (0.088 mol) of 4-dimethylaminopyridine and 239 g of methanol and the mixture was aged for 20 hours under reflux. After cooling, the reaction solution was neutralized with 8.0 g (0.133 mol) of glacial acetic acid, and precipitated by pouring into a large amount of water. The precipitated polymer was dissolved in acetone, then, poured into a large amount of water to cause precipitation. This operation was repeated three times in total, to effect purification. The amount of the resulted copolymer of 2-ethyl-2-adamentyl methacrylate and p-hydroxystyrene was 102.8 g. The weight-average molecular weight was about 8200, the degree of dispersion was 1.68 (GPC method: reduced by polystyrene), and the copolymerization ratio was determined to be about 30:70 by a nuclear magnetic resonance (13C-NMR) spectrometer. This resin is called resin A6.

後処理

  1. temperatureunder reflux
  2. temperatureAfter cooling
  3. customprecipitated
  4. additionby pouring into a large amount of water
  5. dissolutionThe precipitated polymer was dissolved in acetone
  6. additionpoured into a large amount of water
  7. customprecipitation
  8. custompurification

出典と根拠

ORDレコード
ord-7b4ba0d1c5034139a1b4072b94c52353
出典データセット
uspto-grants-2004_02
特許番号
US06689531B2

関連ノート

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