O-Xylene → 2-[3-(3,5-Ditert-butyl-4-hydroxyphenyl)propanoylamino]ethyl 3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoate
反応式
[C:1]([C:5]1[CH:6]=[C:7]([CH2:16][CH2:17][C:18]([NH:20][CH2:21][CH2:22][OH:23])=[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].[C:24]([C:28]1[CH:29]=[C:30]([CH2:39][CH2:40][C:41](O)=[O:42])[CH:31]=[C:32]([C:35]([CH3:38])([CH3:37])[CH3:36])[C:33]=1[OH:34])([CH3:27])([CH3:26])[CH3:25].C1(C)C(C)=CC=CC=1>CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-].[Ti+4].O>[C:35]([C:32]1[CH:31]=[C:30]([CH2:39][CH2:40][C:41]([O:23][CH2:22][CH2:21][NH:20][C:18](=[O:19])[CH2:17][CH2:16][C:7]2[CH:6]=[C:5]([C:1]([CH3:2])([CH3:3])[CH3:4])[C:10]([OH:11])=[C:9]([C:12]([CH3:14])([CH3:15])[CH3:13])[CH:8]=2)=[O:42])[CH:29]=[C:28]([C:24]([CH3:26])([CH3:25])[CH3:27])[C:33]=1[OH:34])([CH3:38])([CH3:36])[CH3:37]参加物
6
反応物 3
生成物 1
試薬・触媒・溶媒 2
実験手順
A mixture of 32 g (0.1 mole) of 3-(3,5-di-tert-butyl-4-hydroxyphenyl)-N-(2-hydroxyethyl)propionamide, 27 g (0.1 mole) of 3(3,5-di-tert-butyl-4-hydroxyphenyl)propionic acid, 1 g Tyzor TBT catalyst and 100 ml xylene was refluxed at 150° until evolution of water ceased. In the course of four hours, two ml water was collected in the Stark & Dean trap. The xylene was removed by vacuum stripping. The title compound (54 g) was recrystallized from a toluene/hexane mixture. It melted at 151°-154° C.
後処理
- customIn the course of four hours, two ml water was collected in the Stark & Dean trap
- customThe xylene was removed by vacuum stripping
- customThe title compound (54 g) was recrystallized from a toluene/hexane mixture
出典と根拠
- ORDレコード
- ord-007e9ef1c46b493896077fb2ad14a8bb
- 出典データセット
- uspto-grants-1981_12
- 特許番号
- US04305868
反応ノート
読み込み中…