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Toluene → 2-(Benzotriazol-2-yl)-4-methyl-6-(2-hydroxy-3-benzoyl-6-methoxybenzyl)phenol

HRID 273900
ノート
印刷プレビュー

反応式

HRID 273900 の反応式
[OH:1][C:2]1[C:7]([CH2:8]N(CC)CC)=[CH:6][C:5]([CH3:14])=[CH:4][C:3]=1[N:15]1[N:19]=[C:18]2[CH:20]=[CH:21][CH:22]=[CH:23][C:17]2=[N:16]1.[OH:24][C:25]1[CH:38]=[C:37]([O:39][CH3:40])[CH:36]=[CH:35][C:26]=1[C:27]([C:29]1[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=1)=[O:28].C[O-].[Na+].C1(C)C=CC=CC=1>CO>[N:16]1[N:15]([C:3]2[CH:4]=[C:5]([CH3:14])[CH:6]=[C:7]([CH2:8][C:38]3[C:37]([O:39][CH3:40])=[CH:36][CH:35]=[C:26]([C:27](=[O:28])[C:29]4[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=4)[C:25]=3[OH:24])[C:2]=2[OH:1])[N:19]=[C:18]2[CH:20]=[CH:21][CH:22]=[CH:23][C:17]=12
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 1140TolueneHCID 46322-Hydroxy-4-methoxybenzophenoneHCID 10942334Sodium MethoxideHCID 159190222-(2-Hydroxy-3-diethylaminomethyl-5-methylphenyl)-2H-benzotriazole

生成物 1

HCID 199172652-(Benzotriazol-2-yl)-4-methyl-6-(2-hydroxy-3-benzoyl-6-methoxybenzyl)phenol収率 68.7%

試薬・触媒・溶媒 1

HCID 887
Methanol
溶媒

反応条件

温度
130 °C

実験手順

2-(2-Hydroxy-3-diethylaminomethyl-5-methylphenyl)-2H-benzotriazole (20.0 g, 0.064 tool), 2-hydroxy-4-methoxybenzophenone (14.7 g, 0,064 mol), and sodium methoxide (1.0 g, 25% in methanol) are charged to a reaction flask. The mixture is heated to 130° C. and held at this temperature for 20 hours with agitation under a nitrogen flow. At that time, the product is identified using thin layer chromatography, with toluene as the mobile phase. To the brown-yellow solid is added hot methanol. The yellow solids are vacuum filtered and triturated twice using methanol, yielding 20.6 g product. To remove the yellow color, the solids are dissolved in hot toluene, and silica gel is introduced. The silica gel is gravity filtered hot. The toluene is removed by vacuum distillation, yielding 12.1 g of the title compound as a pale yellow solid, m.p. 206°-209° C.

後処理

  1. filtrationfiltered
  2. customtriturated twice using methanol

出典と根拠

ORDレコード
ord-16b52211b7e6495ebc7ee76747d44aa2
出典データセット
uspto-grants-1995_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05387691

反応ノート

読み込み中…

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