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

HRID 249225

반응식

HRID 249225 반응식
[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]

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 811Itaconic acidHCID 6581Acrylic Acid

생성물 1

HCID 1615092-Methylidenebutanedioic acid--prop-2-enoic acid (1/1)수율 296.4%

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
55 °C

실험 절차

Acrylic acid (20.000 g, 0.27755 mole), itaconic acid (4.0121 g, 0.038386 mole), Wako V-50 (0.0837 g, 0.308 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 is 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 with molecular weight cut-off at 3500) to remove any unreacted monomers. The dialyzed solution is freeze dried to give 23.00 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 --0.1683), is 896,100.

후처리

  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. temperatureis maintained 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 with molecular weight cut-off at 3500)
  8. customto remove any unreacted monomers
  9. customdried

출처 및 근거

ORD 기록
ord-1f30a51eadaf483e8bf82aa0e389c56b
출처 데이터셋
uspto-grants-1993_05
특허 번호
US05213789

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