Toluene → 2-(5-Chloro-2H-benzotriazol-2-yl)-4-methyl-phenol

HRID 334836

反応式

HRID 334836 の反応式
C([C:5]1[CH:10]=[C:9]([CH3:11])[CH:8]=[C:7]([N:12]2[N:16]=[C:15]3[CH:17]=[CH:18][C:19]([Cl:21])=[CH:20][C:14]3=[N:13]2)[C:6]=1[OH:22])(C)(C)C.C1(C)C=CC=CC=1>>[Cl:21][C:19]1[CH:18]=[CH:17][C:15]2=[N:16][N:12]([C:7]3[CH:8]=[C:9]([CH3:11])[CH:10]=[CH:5][C:6]=3[OH:22])[N:13]=[C:14]2[CH:20]=1

参加物

3

反応物 2

HCID 1140TolueneHCID 62531Tinuvin

生成物 1

HCID 131302032-(5-Chloro-2H-benzotriazol-2-yl)-4-methyl-phenol収率 85.1%

実験手順

To a solution of 2-tert-Butyl-6-(5-chloro-2H-benzotriazol-2-yl)-4-methyl-phenol (50.0 g, 158 mmol) in toluene (700 ml) aluminium trichloride (42.2 g, 317 mmol) is added at 80° C. and the reaction mixture is stirred for 30 minutes, cooled to room temperature and slowly poured on crushed ice. The aqueous phase is extracted with ethyl acetate. The organic layer is washed with water, dried over sodium sulphate, filtered and evaporated to dryness. The crude product is purified by column chromatography (ethyl acetate/heptane 1:12) to yield 34.9 g of 2-(5-Chloro-2H-benzotriazol-2-yl)-4-methyl-phenol.

後処理

  1. additionslowly poured
  2. customon crushed ice
  3. extractionThe aqueous phase is extracted with ethyl acetate
  4. washThe organic layer is washed with water
  5. dry with materialdried over sodium sulphate
  6. filtrationfiltered
  7. customevaporated to dryness
  8. customThe crude product is purified by column chromatography (ethyl acetate/heptane 1:12)

出典と根拠

ORDレコード
ord-3850ab0b2d26406f9b006cdc8f4462f5
出典データセット
uspto-grants-2014_11
特許番号
US08883829B2

関連ノート

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