2-Propenoic acid, 3-hydroxypropyl ester → Isopropenylphosphonic Acid Hydroxypropylacrylate

HRID 543452

반응식

HRID 543452 반응식
[OH:1][CH2:2][CH2:3][CH2:4][O:5][C:6](=[O:9])[CH:7]=[CH2:8].[C:10]([P:13](=[O:16])([OH:15])[OH:14])([CH3:12])=[CH2:11]>O>[C:10]([P:13](=[O:14])([OH:16])[OH:15])([CH3:12])=[CH2:11].[OH:1][CH2:2][CH2:3][CH2:4][O:5][C:6](=[O:9])[CH:7]=[CH2:8]

참가 물질

4

반응물 2

HCID 331012-Propenoic acid, 3-hydroxypropyl esterHCID 557541Isopropenylphosphonic acid

생성물 1

HCID 86739384Isopropenylphosphonic Acid Hydroxypropylacrylate

시약·촉매·용매 1

HCID 962Water용매

실험 절차

To a 500 ml resin kettle equipped with a mechanical stirrer, thermometer, pressure compensated addition funnel, and reflux condenser, was added hydroxypropylacrylate (26.6 g; 0.2 mole). Isopropenyl phosphonic acid (25.4 g; 0.2 mole) was dissolved in 154.2 g water and added rapidly to the kettle. The reaction mixture was then sparged with nitrogen for 1/2 hour. Ammonium persulfate (6 g) was added and the nitrogen sparge continued for an additional 1/2 hour. The mixture was heated to reflux for 2 hours. An additional 6 g of ammonium persulfate was added. The mixture was then refluxed for an additional 2 hours. There was a definite increase in viscosity after the second addition of ammonium persulfate. The yellow product had a pH of 1.00 and was tested without further purification. A 31PMR spectrum showed broad polymer absorptions centered at δ=-32.9 and -34.7 ppm and a small amount of monomer at δ=-19.0 ppm. There was also a trace of inorganic phosphate.

후처리

  1. additionaddition funnel
  2. temperaturereflux condenser
  3. additionadded rapidly to the kettle
  4. customThe reaction mixture was then sparged with nitrogen for 1/2 hour
  5. additionAmmonium persulfate (6 g) was added
  6. customthe nitrogen sparge
  7. temperatureThe mixture was heated
  8. temperatureto reflux for 2 hours
  9. additionAn additional 6 g of ammonium persulfate was added
  10. temperatureThe mixture was then refluxed for an additional 2 hours
  11. temperaturea definite increase in viscosity
  12. additionafter the second addition of ammonium persulfate
  13. customwas tested without further purification

출처 및 근거

ORD 기록
ord-4087c4d0bcd74e09a9777e9d86975877
출처 데이터셋
uspto-grants-1984_05
특허 번호
US04446028

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