O-Xylene → 2-(Lauramido)ethyl 3-(3,5-di-tert-butyl-4-hydroxyphenyl)-propionate

HRID 1659897

반응식

HRID 1659897 반응식
[OH:1][CH2:2][CH2:3][NH:4][C:5](=[O:17])[CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH3:16].[C:18]([C:22]1[CH:23]=[C:24]([CH2:33][CH2:34][C:35](O)=[O:36])[CH:25]=[C:26]([C:29]([CH3:32])([CH3:31])[CH3:30])[C:27]=1[OH:28])([CH3:21])([CH3:20])[CH3:19].C1(C)C(C)=CC=CC=1>CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-].[Ti+4].O>[C:29]([C:26]1[CH:25]=[C:24]([CH2:33][CH2:34][C:35]([O:1][CH2:2][CH2:3][NH:4][C:5](=[O:17])[CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH3:16])=[O:36])[CH:23]=[C:22]([C:18]([CH3:20])([CH3:19])[CH3:21])[C:27]=1[OH:28])([CH3:32])([CH3:30])[CH3:31]

참가 물질

6

반응물 3

HCID 7237O-XyleneHCID 8899Lauric acid monoethanolamideHCID 883893-(3',5'-Di-tert-butyl-4'-hydroxyphenyl)propionic acid

생성물 1

HCID 205584872-(Lauramido)ethyl 3-(3,5-di-tert-butyl-4-hydroxyphenyl)-propionate

시약·촉매·용매 2

HCID 21801Titanium tetrabutoxide촉매HCID 962Water용매

반응 조건

온도
-10 °C

실험 절차

A mixture of 13.9 g (0.055 mole) N-(2-hydroxyethyl)lauramide, 13.9 g (0.05 mole) 3(3,5-di-tert-butyl-4-hydroxyphenyl)propionic acid, 0.5 g Tyzor TBT catalyst and 100 ml xylene was refluxed until evolution of water ceased (3 hours). The xylene was removed by vacuum stripping. The residue was taken up in acetonitrile. White crystals separated upon cooling at about -10° C. The acetonitrile was decanted and the recrystallization was repeated. The last traces of acetonitrile were removed under vacuum, and the title product thus obtained was a yellow oil at room temperature.

후처리

  1. custom(3 hours)
  2. customThe xylene was removed by vacuum stripping
  3. customWhite crystals separated
  4. customThe acetonitrile was decanted
  5. customthe recrystallization
  6. customThe last traces of acetonitrile were removed under vacuum

출처 및 근거

ORD 기록
ord-b3ff0b9801c74ba8b367eef2ae104c85
출처 데이터셋
uspto-grants-1981_12
특허 번호
US04305868

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