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Sulfuric Acid → Sodium styrenesulfonate 2-(amino)ethylmethacrylate

HRID 1193471
ノート
印刷プレビュー

反応式

HRID 1193471 の反応式
[CH:1]([S:9]([O-:12])(=[O:11])=[O:10])=[CH:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1.[Na+:13].[NH2:14][CH2:15][CH2:16][O:17][C:18](=[O:22])[C:19]([CH3:21])=[CH2:20].S(=O)(=O)(O)O.C(ON(OC(=O)C)CCN(OC(=O)C)OC(=O)C)(=O)C.[Na].[Na]>O>[C:18]([O:17][CH2:16][CH2:15][NH2:14])(=[O:22])[C:19]([CH3:21])=[CH2:20].[CH:1]([S:9]([O-:12])(=[O:10])=[O:11])=[CH:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1.[Na+:13]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 1118Sulfuric AcidHCID 754962-AminoethylmethacrylateHCID 53627496Sodium styrenesulfonateHCID 86742785Disodium ethylenediamine tetraacetate

生成物 1

HCID 86741551Sodium styrenesulfonate 2-(amino)ethylmethacrylate収率 11%

試薬・触媒・溶媒 1

HCID 962
Water
溶媒

反応条件

温度
65 °C

実験手順

A solution of 35 g of sodium styrenesulfonate and 14 g of 35% 2-(amino)ethylmethacrylate.HC1 solution in 200 ml of water was prepared. The pH was adjusted to 3.5 using 1N sulfuric acid, and 0.1 g disodium ethylenediamine tetraacetate was added to the above solution. The solution was then N2 sparged for 30 minutes and heated to 65° C. 3 g of 4,4'-azobis(4-cyanovaleric acid) were then added, and the solution maintained at 65° C. for 6 hours. The reactants were poured into 1 liter of acetone, the acetone was decanted off, and methanol added. This mixture was allowed to stand overnight, followed by filtration and methanol-washing. Vacuum oven drying gave 40 g of a 11% 2-(amino)ethyl methacrylate/sodium styrenesulfonate copolymer, a white solid.

後処理

  1. additionwas added to the above solution
  2. customN2 sparged for 30 minutes
  3. addition3 g of 4,4'-azobis(4-cyanovaleric acid) were then added
  4. temperaturethe solution maintained at 65° C. for 6 hours
  5. additionThe reactants were poured into 1 liter of acetone
  6. customthe acetone was decanted off
  7. additionmethanol added
  8. filtrationfollowed by filtration and methanol-
  9. washwashing
  10. customVacuum oven drying

出典と根拠

ORDレコード
ord-7fcdb642f9d94700980f0d5de5fd7c86
出典データセット
uspto-grants-1989_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04810624

反応ノート

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