Acetic Acid → Prop-2-enimidic acid--2-(dimethylamino)ethyl 2-methylprop-2-enoate (1/1)

HRID 27831

반응식

HRID 27831 반응식
C(O)(=O)C.[C:5]([O:10][CH2:11][CH2:12][N:13]([CH3:15])[CH3:14])(=[O:9])[C:6]([CH3:8])=[CH2:7].[C:16]([NH2:20])(=[O:19])[CH:17]=[CH2:18].CCCCCCCC/C=C\CCCCCCCC(OCC(O)[C@H]1OC[C@H](O)[C@H]1O)=O>O>[C:16]([NH2:20])(=[O:19])[CH:17]=[CH2:18].[CH3:8][C:6]([C:5]([O:10][CH2:11][CH2:12][N:13]([CH3:15])[CH3:14])=[O:9])=[CH2:7]

참가 물질

6

반응물 4

HCID 176Acetic AcidHCID 6579AcrylamideHCID 17869(Dimethylamino)ethyl methacrylateHCID 70693544Span #80 (Sorbitan monooleate)

생성물 1

HCID 160008Prop-2-enimidic acid--2-(dimethylamino)ethyl 2-methylprop-2-enoate (1/1)

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
50 °C

실험 절차

To a solution of 41.9 grams of glacial acetic acid in 350 grams of tap water is added 109.6 grams of dimethylaminoethyl methacrylate (DMAEMA), followed by 148.7 grams of acrylamide (AM). The monomer solution pH is 7.0. It is added slowly to a rapidly stirred solution of 30 grams of sorbitan monooleate (SMO) in 320 grams of Shellflex 131. The resulting emulsion is sparged with nitrogen, warmed to 50° C. and treated with a solution 0.10 grams of bis azoisobutyronitrile (DuPont VAZO) in 2 milliliters of benzene. The polymerization began after a 30 minute induction period. Samples are withdrawn every hour and the residual monomer content determined by gas-liquid chromatography. After 5 hours the DMAEMA had completely disappeared and 20% of the acrylamide was recovered by GLC. This indicates that ≈60% of the DMAEMA has been quaternized by the acrylamide. A small portion of the monomer solution was stored at 25° C. for 24 hours. The NMR spectrum showed that 50% of the DMAEMA had been quaternized.

후처리

  1. customThe resulting emulsion is sparged with nitrogen
  2. additiontreated with a solution 0.10 grams of bis azoisobutyronitrile (DuPont VAZO) in 2 milliliters of benzene
  3. customSamples are withdrawn every hour
  4. waitAfter 5 hours the DMAEMA had completely disappeared
  5. custom20% of the acrylamide was recovered by GLC
  6. waitA small portion of the monomer solution was stored at 25° C. for 24 hours

출처 및 근거

ORD 기록
ord-c92864c272fa404dbedba6d4a51e652d
출처 데이터셋
uspto-grants-1980_09
특허 번호
US04224150

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