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Ethyl Lactate → Hydroxystyrene

HRID 1940465
ノート
印刷プレビュー

反応式

HRID 1940465 の反応式
[CH3:1][CH2:2][CH2:3][CH2:4][CH2:5]C.[C:7]([O:12]CC)(=O)[CH:8]([CH3:10])O>>[OH:12][CH:7]=[CH:8][C:10]1[CH:5]=[CH:4][CH:3]=[CH:2][CH:1]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

3

反応物 2

HCID 7344Ethyl LactateHCID 8058Hexane

生成物 1

HCID 138202Hydroxystyrene

実験手順

A solution prepared by dissolving 10.0 g of a poly(hydroxystyrene) resin having a weight-average molecular weight of 20000 with a dispersion of the molecular weight distribution Mw /Mn of 1.1 (VP-20000, a product by Nippon Soda Co.), which contained a few % by weight or less of unpolymerized monomer and oligomers having a molecular weight smaller than 1000, in 40 g of ethyl lactate was taken in a separatory funnel and admixed with 150 g of n-hexane and the mixture was thoroughly shaken followed by standing to effect phase separation into an upper layer of the n-hexane solution and lower layer of the ethyl lactate solution. The n-hexane solution as the upper layer was discarded and the ethyl lactate solution as the lower layer was again admixed with 150 g of n-hexane followed by vigorous shaking of the mixture. This fractionating extraction with n-hexane was repeatedly undertaken four times and the finally obtained ethyl lactate solution was subjected to replacement of solvent with methyl alcohol by repeating evaporation of ethyl lactate and addition of methyl alcohol. The thus obtained methyl alcohol solution was added dropwise into a large volume of water to effect precipitation of the polymer which was collected, washed with pure water and dried to give a poly(hydroxystyrene) resin substantially free from unpolymerized hydroxystyrene monomer and oligomers having a molecular weight smaller than 1000 as confirmed by the GPC method. Since the content of the low molecular weight fractions in the starting resin was relatively low, no significant changes were found in the weight-average molecular weight and in the dispersion of the molecular weight distribution.

後処理

  1. customA solution prepared
  2. customphase separation into an upper layer of the n-hexane solution and lower layer of the ethyl lactate solution
  3. stirringby vigorous shaking of the mixture
  4. extractionThis fractionating extraction with n-hexane
  5. customevaporation of ethyl lactate and addition of methyl alcohol
  6. additionThe thus obtained methyl alcohol solution was added dropwise into a large volume of water
  7. customprecipitation of the polymer which
  8. customwas collected
  9. washwashed with pure water
  10. customdried

出典と根拠

ORDレコード
ord-2630120bd99b45d8b5333318e0bf965d
出典データセット
uspto-grants-1997_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05700625

反応ノート

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