Acrylic Acid → Itaconamide acrylic acid

HRID 1633391

反応式

HRID 1633391 の反応式
[C:1]([OH:5])(=[O:4])[CH:2]=[CH2:3].[C:6]([NH2:14])(=[O:13])[C:7]([CH2:9][C:10]([NH2:12])=[O:11])=[CH2:8].Cl.N(C(C(=N)N)(C)C)=NC(C(=N)N)(C)C>O>[C:6]([NH2:14])(=[O:13])[C:7]([CH2:9][C:10]([NH2:12])=[O:11])=[CH2:8].[C:1]([OH:5])(=[O:4])[CH:2]=[CH2:3]

参加物

5

反応物 3

HCID 6581Acrylic AcidHCID 84924Propanimidamide, 2,2'-(1,2-diazenediyl)bis[2-methyl-, hydrochloride (1:?)HCID 239162Itaconamide

生成物 1

HCID 86739744Itaconamide acrylic acid

試薬・触媒・溶媒 1

HCID 962Water溶媒2 回

実験手順

In a 50 ml. round bottom blask equipped with a stopcock adapter were placed 216 mg. (3 equivalents) of acrylic acid, 128 mg. (1 equivalent) of itaconamide, prepared as described in Example 2, 10 mg. of 2,2'-azobis (2-amidinopropane) hydrochloride (available from Crescent Chemical Co., Inc., Hauppauge, N.Y. under the tradename V-50), and 10 ml. of water. The flask was evacuated and sealed as described in Example 3 and placed in a 65° C. bath for 10 days. The reaction mixture was then cooled to room temperature and the water evaporated by blowing a stream of air across the surface. The residue was dissolved in 50 ml. of water and the solution subjected to pressure filtration in an Amicon Cell #402 (available from Amicon Corp., Lexington, MA) fitted with an Amicon Filter UM-2 having a molecular weight cut-off of 1000. A concentrated polymer solution was obtained which was diluted with water and the pressure filtration process repeated. This process was repeated several times until essentially all low molecular weight impurities were removed. The resultant copolymer solution was evaporated to dryness to yield a copolymer of itaconamide/acrylic acid as a white solid. Infrared spectral analysis was consistent with the copolymer structure. Elemental analysis of nitrogen content indicated a molar percentage of itaconamide in the copolymer of 24%.

後処理

  1. customround bottom blask equipped with a stopcock adapter
  2. customThe flask was evacuated
  3. customsealed
  4. customplaced in a 65° C.
  5. customfor 10 days
  6. customthe water evaporated
  7. dissolutionThe residue was dissolved in 50 ml
  8. filtrationof water and the solution subjected to pressure filtration in an Amicon Cell #402 (available from Amicon Corp., Lexington, MA)
  9. customfitted with an Amicon
  10. filtrationFilter UM-2
  11. customA concentrated polymer solution was obtained which
  12. filtrationthe pressure filtration process
  13. customwere removed
  14. customThe resultant copolymer solution was evaporated to dryness

出典と根拠

ORDレコード
ord-2c575f51840c48fd9b0811b27b1246a3
出典データセット
uspto-grants-1984_10
特許番号
US04480125

関連ノート

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