Hydrochloric Acid → 3-(5-Chlorobenzotriazol-2-yl)-5-tert-butyl-4-hydroxyhydrocinnamic acid

HRID 1779526

反応式

HRID 1779526 の反応式
[Cl:1][C:2]1[CH:34]=[CH:33][C:5]2=[N:6][N:7]([C:9]3[CH:10]=[C:11]([CH2:20][CH2:21][C:22]([O:24]CCCCCCCC)=[O:23])[CH:12]=[C:13]([C:16]([CH3:19])([CH3:18])[CH3:17])[C:14]=3[OH:15])[N:8]=[C:4]2[CH:3]=1.[OH-].[Na+].Cl>CC(C)=O>[Cl:1][C:2]1[CH:34]=[CH:33][C:5]2=[N:6][N:7]([C:9]3[CH:10]=[C:11]([CH2:20][CH2:21][C:22]([OH:24])=[O:23])[CH:12]=[C:13]([C:16]([CH3:17])([CH3:18])[CH3:19])[C:14]=3[OH:15])[N:8]=[C:4]2[CH:3]=1

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 174297Octyl 5-tert-butyl-3-(5-chloro-2H-benzotriazole-2-yl)-4-hydroxybenzenepropionate

生成物 1

HCID 180087183-(5-Chlorobenzotriazol-2-yl)-5-tert-butyl-4-hydroxyhydrocinnamic acid

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

225 g (0.46 mol) of octyl 3-(5-chloro-2H-benzotriazole-2-yl)-5-(1,1-dimethylethyl)-4-hydroxy-benzene propanate manufactured by CIBA GEIGY INC. under the trade name of "TINUVIN 109" were dissolved in 700 ml of acetone. To the resulting solution were added 600 ml of a 2N aqueous solution of sodium hydroxide followed by agitation at room temperature for 24 hours. Then, 650 ml of a 2N aqueous solution of hydrochloric acid was added to give an acidic solution and an insolubilized product was filtered off and rinsed with distilled water until the filtrate turned neutral. After vacuum-drying the product, it was recrystallized from toluene to give 3-(5-chloro-2H-benzotriazol-2-yl)-5-(1,1-dimethylethyl)-4-hydroxy benzene propanoic acid, referred to hereinafter as a precursor (3).

後処理

  1. customto give an acidic solution
  2. filtrationan insolubilized product was filtered off
  3. washrinsed with distilled water until the filtrate
  4. customAfter vacuum-drying the product, it
  5. customwas recrystallized from toluene

出典と根拠

ORDレコード
ord-7ef518848a16424689b5cada6f21f11a
出典データセット
uspto-grants-1997_05
特許番号
US05627227

関連ノート

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