Hydrochloric Acid → 2-Methylidenebutanedioic acid--prop-2-enoic acid (1/1)

HRID 249229

反応式

HRID 249229 の反応式
[C:1]([OH:5])(=[O:4])[CH:2]=[CH2:3].[C:6]([OH:14])(=[O:13])[C:7]([CH2:9][C:10]([OH:12])=[O:11])=[CH2:8].Cl>O>[CH2:3]=[CH:2][C:1]([OH:5])=[O:4].[CH2:8]=[C:7]([C:6]([OH:14])=[O:13])[CH2:9][C:10]([OH:12])=[O:11]

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 811Itaconic acidHCID 6581Acrylic Acid

生成物 1

HCID 1615092-Methylidenebutanedioic acid--prop-2-enoic acid (1/1)収率 48.1%

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
55 °C

実験手順

Acrylic acid (21.11 g, 0.2930 mole), itaconic acid (2.0061 g, 15.420 millimole), Wako V-50 (0.0837 g, 0.309 millimole), and 150 ml of water, which has been acidified to pH 2.0 with hydrochloric acid, are added to a 250 ml three-necked round-bottomed flask. The necks are fitted with a thermometer, a stopper, and a gas inlet/outlet adapter capable of bubbling gas through a liquid in the flask and venting it. The solution is deaerated by passage of nitrogen gas and is then placed under an atmosphere of argon. The solution is heated to 55° C. and maintained at this temperature for 15 hours. The viscous solution of copolymer is cooled to ambient temperature and is dialyzed against distilled water overnight (Spectrapor 3 tubing as in the foregoing Examples) to remove any unreacted monomers and then freeze dried to give 1.5 g of poly(acrylic acid-itaconic acid) copolymer as a colorless solid. The mass average molecular weight, as determined by low angle laser light scattering in 0.2 Molar sodium chloride in water (refractive index=1.3344, dn /dc =0.1670), is 925,000.

後処理

  1. additionare added to a 250 ml three-necked round-bottomed flask
  2. customThe necks are fitted with a thermometer
  3. customa stopper, and a gas inlet/outlet adapter capable of bubbling gas through a liquid in the flask
  4. temperaturemaintained at this temperature for 15 hours
  5. temperatureThe viscous solution of copolymer is cooled to ambient temperature
  6. customis dialyzed
  7. distillationagainst distilled water overnight (Spectrapor 3 tubing as in the foregoing Examples)
  8. customto remove any unreacted monomers
  9. customfreeze dried

出典と根拠

ORDレコード
ord-c2d47e12fcbf4ff283008e150843cfba
出典データセット
uspto-grants-1993_05
特許番号
US05213789

関連ノート

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