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

HRID 334836

반응식

HRID 334836 반응식
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

참가 물질

3

반응물 2

HCID 1140TolueneHCID 62531Tinuvin

생성물 1

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

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-3850ab0b2d26406f9b006cdc8f4462f5
출처 데이터셋
uspto-grants-2014_11
특허 번호
US08883829B2

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