Water → Butyl prop-2-enoate--methyl 2-methylprop-2-enoate (1/1)

HRID 748553

反応式

HRID 748553 の反応式
O.[C:2]([O:6][CH2:7][CH2:8][CH2:9][CH3:10])(=[O:5])[CH:3]=[CH2:4].[C:11](=O)([O-])[O-].[Ca+2]>C(OC)(=O)C(C)=C.N(C(C#N)(C)CCC(O)=O)=NC(C#N)(C)CCC(O)=O>[C:2]([O:6][CH3:7])(=[O:5])[C:3]([CH3:11])=[CH2:4].[C:2]([O:6][CH2:7][CH2:8][CH2:9][CH3:10])(=[O:5])[CH:3]=[CH2:4]

参加物

6

反応物 3

HCID 962WaterHCID 8846Butyl AcrylateHCID 10112Calcium Carbonate

生成物 1

HCID 62802Butyl prop-2-enoate--methyl 2-methylprop-2-enoate (1/1)

試薬・触媒・溶媒 2

HCID 929384,4-Azobis(4-cyanovaleric acid)触媒HCID 6658Methyl Methacrylate溶媒2 回

実験手順

(wherein Me represents methyl and Ph represents phenyl), was dissolved in 3.0 g of methyl methacrylate as a monomer, and the solution was added into the reactor. After 20 minutes, as a polymerization initiator, 555 mg of 4,4′-azobis(4-cyanovaleric acid) together with 12 g of distilled water was added into the reactor. Stirring was performed at 80° C. for 20 minutes, and then 52.0 g of methyl methacrylate was dripped from the dropping funnel for over 90 minutes. After 30 minutes, 61.0 g of n-butyl acrylate as a monomer was dripped from the dropping funnel for over 1 hour. Stirring was performed at 80° C. for 6 hours, and the emulsion was salted out with calcium carbonate, followed by washing with distilled water. Thereby, 94.1 g of a methyl methacrylate-n-butyl acrylate diblock copolymer was produced. GPC confirmed that in the polymer, Mw=59,800, Mn=44,400, and Mw/Mn=1.35. 1H NMR analysis confirmed that the weight ratio of the poly(methyl methacrylate) portion to the poly(n-butyl acrylate) portion was 48:52, and that thiocarbonylthio groups were introduced at the poly(n-butyl acrylate) ends with an introduction rate of 84%.

後処理

  1. additionthe solution was added into the reactor
  2. waitwas performed at 80° C. for 20 minutes
  3. customwas dripped from the dropping funnel for over 90 minutes
  4. waitAfter 30 minutes
  5. customwas dripped from the dropping funnel for over 1 hour
  6. stirringStirring
  7. waitwas performed at 80° C. for 6 hours
  8. washby washing with distilled water

出典と根拠

ORDレコード
ord-79d2beca13714bea92273351fdd836a0
出典データセット
uspto-grants-2008_07
特許番号
US07399801B2

関連ノート

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