Glycidyl methacrylate → Quadrol dimethylacrylate

HRID 477719

반응식

HRID 477719 반응식
[C:1](O[CH2:7][CH:8]1[O:10][CH2:9]1)(=O)[C:2](C)=[CH2:3].C[O:12]C1C=[CH:17][C:16]([OH:19])=[CH:15]C=1.[OH:20][CH:21]([CH3:31])[CH2:22][NH:23][CH2:24][CH2:25][NH:26][CH2:27][CH:28]([OH:30])[CH3:29]>CO>[CH3:29][CH:28]([OH:30])[CH2:27][N:26]([CH2:9][CH:8]([OH:10])[CH3:7])[CH2:25][CH2:24][N:23]([CH2:17][CH:16]([OH:19])[CH3:15])[CH2:22][CH:21]([OH:20])[CH3:31].[CH3:1][C:2]([CH3:3])=[CH:29][C:28]([O-:30])=[O:12]

참가 물질

5

반응물 3

HCID 7837Glycidyl methacrylateHCID 90154-MethoxyphenolHCID 1029642-Propanol, 1,1'-(1,2-ethanediyldiimino)bis-

생성물 1

HCID 131716219Quadrol dimethylacrylate수율 48%

시약·촉매·용매 1

HCID 887Methanol용매

반응 조건

온도
30 °C

실험 절차

Glycidyl methacrylate (4.8g, 34 mmol) and 4-methoxyphenol (0.13 g) were added to a solution of N,N'-bis-(2-hydroxypropyl)ethylenediamine (IV-a) (3.0 g, 17 mmol) in 80 mL of methanol at 0° C. The mixture was brought to room temperature and maintained for eight days, followed by heating for 24 hours at 30° C. A quantitative yield of a viscous, slightly brown liquid was obtained after removal of the solvent. The product was further purified by dissolving the liquid in water followed by the addition of sodium chloride to saturation. The oil layer was separated, dissol ved in CH2Cl2 and dried over magnesium sulfate. Filtration and removal of solvent yielded Quadrol dimethylacrylate (VII-a) [yield 48 percent: IR(neet):3350(broad OH); 1700 (C=O); 1620(C=C); NMR (CDCl3): δ6.1(s,2H); 5.6(s,2H); 3.8(broad m,8H); 2.6(broad m,12); 2.0(s,6H); 1.1(d,6H)].

후처리

  1. customwas brought to room temperature
  2. temperaturemaintained for eight days
  3. customA quantitative yield of a viscous, slightly brown liquid was obtained
  4. customafter removal of the solvent
  5. customThe product was further purified
  6. dissolutionby dissolving the liquid in water
  7. additionfollowed by the addition of sodium chloride to saturation
  8. customThe oil layer was separated
  9. dry with materialdried over magnesium sulfate
  10. filtrationFiltration and removal of solvent

출처 및 근거

ORD 기록
ord-31f38aca7f7b496987b1ccacf9a723f4
출처 데이터셋
uspto-grants-1989_12
특허 번호
US04889530

연결된 노트

불러오는 중…