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

HRID 1659899ノート

反応式

HRID 1659899 の反応式
[C:1]([C:5]1[CH:6]=[C:7]([CH2:16][CH2:17][C:18]([OH:20])=[O:19])[CH:8]=[C:9]([C:12]([CH3:15])([CH3:14])[CH3:13])[C:10]=1[OH:11])([CH3:4])([CH3:3])[CH3:2].O[CH2:22][CH2:23][NH:24][C:25](=[O:43])[CH2:26][CH2:27][CH2:28][CH2:29][CH2:30][CH2:31][CH2:32][CH2:33][CH2:34][CH2:35][CH2:36][CH2:37][CH2:38][CH2:39][CH2:40][CH2:41][CH3:42].C1(C)C(C)=CC=CC=1>CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-].[Ti+4].O>[C:1]([C:5]1[CH:6]=[C:7]([CH2:16][CH2:17][C:18]([O:20][CH2:22][CH2:23][NH:24][C:25](=[O:43])[CH2:26][CH2:27][CH2:28][CH2:29][CH2:30][CH2:31][CH2:32][CH2:33][CH2:34][CH2:35][CH2:36][CH2:37][CH2:38][CH2:39][CH2:40][CH2:41][CH3:42])=[O:19])[CH:8]=[C:9]([C:12]([CH3:13])([CH3:14])[CH3:15])[C:10]=1[OH:11])([CH3:4])([CH3:2])[CH3:3]

参加物

6

反応物 3

HCID 7237O-XyleneHCID 27902N-StearoylethanolamineHCID 883893-(3',5'-Di-tert-butyl-4'-hydroxyphenyl)propionic acid

生成物 1

HCID 205584912-Stearamidoethyl 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

実験手順

A mixture of 30.6 g (0.11 mole) 3-(3,5-di-tert-butyl-4-hydroxyphenyl)propionic acid, 32.6 g (0.1 mole) N-(2-hydroxyethyl)stearamide, 0.8 g Tyzor TBT, and 100 ml xylene was refluxed for six hours. The water (1.8 ml) was trapped in a Stark & Dean trap. The solution was filtered through Microcel (trademark, synthetic calcium silicate) and the solvent was removed by vacuum stripping. The title compound (51 g) was recrystallized from acrylonitrile. It melted at 52°-55° C.

後処理

  1. temperaturewas refluxed for six hours
  2. filtrationThe solution was filtered through Microcel (trademark, synthetic calcium silicate)
  3. customthe solvent was removed by vacuum stripping
  4. customThe title compound (51 g) was recrystallized from acrylonitrile

出典と根拠

ORDレコード
ord-17febe92b6be438884d353ab4e1d39ed
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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