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

HRID 1659897ノート

反応式

HRID 1659897 の反応式
[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]

参加物

6

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 21801Titanium tetrabutoxide触媒HCID 962Water溶媒

反応条件

温度
-10 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-b3ff0b9801c74ba8b367eef2ae104c85
出典データセット
uspto-grants-1981_12
特許番号
US04305868

反応ノート

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