Ethanol → Triethylene glycol ethoxymalonate methacrylate

HRID 1005495

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HRID 1005495 반응식
[C:1]([O:9]CC)(=[O:8])[CH2:2][C:3]([O:5]CC)=[O:4].P([O-])(O)(O)=O.[K+].C([C:22]1C=C(C)C=C(C(C)(C)C)[C:23]=1[OH:33])(C)(C)C.[C:34]([O:39][CH2:40][CH2:41][O:42][CH2:43][CH2:44][O:45][CH2:46][CH2:47][OH:48])(=[O:38])[C:35]([CH3:37])=[CH2:36].C(O)C>>[C:34]([OH:39])(=[O:38])[C:35]([CH3:37])=[CH2:36].[CH2:23]([O:33][CH:2]([C:3]([OH:5])=[O:4])[C:1]([OH:9])=[O:8])[CH3:22].[CH2:40]([OH:39])[CH2:41][O:42][CH2:43][CH2:44][O:45][CH2:46][CH2:47][OH:48]

참가 물질

6

반응물 5

HCID 702EthanolHCID 7761Diethyl MalonateHCID 314042,6-Di-tert-butyl-4-methylphenolHCID 516951Monobasic potassium phosphateHCID 139080612-(2-(2-Hydroxyethoxy)ethoxy)ethyl 2-methyl-2-propenoate

생성물 1

HCID 86755350Triethylene glycol ethoxymalonate methacrylate

반응 조건

온도
130 °C

실험 절차

The same flask as used in Example 1 was charged with a mixture of 1281.36g (8.0 mol) of diethyl malonate, 4.58g (34 mmol) of potassium dihydrogen phosphate, and 1.95g (0.9 mmol) of 2,6-di-t-butyl-4-methylphenol. After raising the inner teperature to 130° C., 174.48g (0.8 mol) of triethylene glycol monomethacrylate (MA-30 sold by Nippon Nyukazai Co., Ltd.) was added dropwise over 1 hour. After the addition, the mixture was heated at 130° C. for 4 hours. 32.21g (0.7 mol) of ethanol was recovered during the reactio period. Then the mixture was filtered to remove potassium dihydrogen phosphate and evaporated to remove remaiing diethyl malonate. 252.48g (95.0 % of theory) of triethylene glycol ethoxymalonate methacrylate was obtained.

후처리

  1. additionAfter the addition
  2. temperaturethe mixture was heated at 130° C. for 4 hours
  3. filtrationThen the mixture was filtered
  4. customto remove potassium dihydrogen phosphate
  5. customevaporated
  6. customto remove

출처 및 근거

ORD 기록
ord-7a1577caa38643f6b7a1e9ab8e8a28f7
출처 데이터셋
uspto-grants-2000_04
특허 번호
US06054606

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