Acetic Acid → 5-(3',5'-Di-tert.-butyl-4'-hydroxy-phenylethyl)-5-methyl-3-ethoxycarbonylethyl-hydantoin

HRID 1578825노트

반응식

HRID 1578825 반응식
[C:1]([C:5]1[CH:6]=[C:7]([CH2:16][CH2:17][C:18]2([CH3:25])[NH:22][C:21](=[O:23])[NH:20][C:19]2=[O:24])[CH:8]=[C:9]([C:12]([CH3:15])([CH3:14])[CH3:13])[C:10]=1[OH:11])([CH3:4])([CH3:3])[CH3:2].[CH2:26]([O:28][C:29](=[O:32])[CH:30]=[CH2:31])[CH3:27].[OH-].C([N+](C)(C)C)C1C=CC=CC=1.C(O)(=O)C>C(O)C.CO.O>[C:12]([C:9]1[CH:8]=[C:7]([CH2:16][CH2:17][C:18]2([CH3:25])[NH:22][C:21](=[O:23])[N:20]([CH2:31][CH2:30][C:29]([O:28][CH2:26][CH3:27])=[O:32])[C:19]2=[O:24])[CH:6]=[C:5]([C:1]([CH3:2])([CH3:3])[CH3:4])[C:10]=1[OH:11])([CH3:15])([CH3:14])[CH3:13]

참가 물질

8

반응물 4

HCID 176Acetic AcidHCID 8821Ethyl AcrylateHCID 66854Benzyltrimethylammonium hydroxideHCID 214162765-(3'5'-Di-tert-butyl-4'-hydroxyphenylethyl)-5-methylhydantoin

생성물 1

HCID 214162965-(3',5'-Di-tert.-butyl-4'-hydroxy-phenylethyl)-5-methyl-3-ethoxycarbonylethyl-hydantoin수율 74.6%

시약·촉매·용매 3

HCID 702Ethanol용매HCID 887Methanol용매HCID 962Water용매

실험 절차

30 g (0.087 mol) of 5-(3',5'-di-tert.-butyl-4'-hydroxyphenylethyl)-5-methyl-hydantoin and 13.1 g (0.131 mol) of acrylic acid ethyl ester are dissolved in 100 ml of ethanol, 2 ml of a 40% strength solution of benzyl-trimethyl-ammonium hydroxide in methanol are added and the mixture is heated under reflux for 12 hours, whilst stirring. Thereafter it is neutralised with glacial acetic acid, diluted with 50 ml of water and cooled whilst stirring. The precipitate formed is filtered off, washed with 50% strength ethanol and recrystallised from 70% strength alcohol. 29 g of 5-(3',5'-di-tert.-butyl-4'-hydroxy-phenylethyl)-5-methyl-3-ethoxycarbonylethyl-hydantoin of melting point 100°C are thus obtained. (Stabiliser No. 9).

후처리

  1. temperaturethe mixture is heated
  2. temperatureunder reflux for 12 hours
  3. temperaturecooled
  4. stirringwhilst stirring
  5. customThe precipitate formed
  6. filtrationis filtered off
  7. washwashed with 50% strength ethanol
  8. customrecrystallised from 70% strength alcohol

출처 및 근거

ORD 기록
ord-0e2a991b5c314de7a05105e34b685d81
출처 데이터셋
uspto-grants-1976_02
특허 번호
US03939175

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