Sulfuric Acid → Phenol, 2-(2H-benzotriazol-2-yl)-4-(1,1-dimethylethyl)-

HRID 1763177

반응식

HRID 1763177 반응식
O=C[C@@H]([C@H]([C@@H]([C@@H](CO)O)O)O)O.[OH:13][C:14]1[CH:19]=[CH:18][C:17]([C:20]([CH3:23])([CH3:22])[CH3:21])=[CH:16][C:15]=1[N:24]1[N+:28]([O-])=[C:27]2[CH:30]=[CH:31][CH:32]=[CH:33][C:26]2=[N:25]1.C1C2C(=O)C3C(=CC=CC=3)CC=2C=CC=1.S(=O)(=O)(O)O>C1C2C(=O)C3C(=CC=CC=3)C=2C=CC=1>[OH:13][C:14]1[CH:19]=[CH:18][C:17]([C:20]([CH3:23])([CH3:22])[CH3:21])=[CH:16][C:15]=1[N:24]1[N:28]=[C:27]2[CH:30]=[CH:31][CH:32]=[CH:33][C:26]2=[N:25]1

참가 물질

6

반응물 4

HCID 1118Sulfuric AcidHCID 7018AnthroneHCID 107526(2R,3S,4R,5R)-2,3,4,5,6-pentahydroxyhexanalHCID 139071722-(2-hydroxy-5-t-butylphenyl)benzotriazole-N-oxide

생성물 1

HCID 76605Phenol, 2-(2H-benzotriazol-2-yl)-4-(1,1-dimethylethyl)-

시약·촉매·용매 1

HCID 10241Fluorenone촉매

실험 절차

9-fluorenone 0.7 g was then added to the reaction liquor thus obtained, and the liquor was heated to 55°~60° C. Thereafter, glucose 6.0 g was added to the reaction liquor over 30 minutes, and the reaction was conducted at 75° C. (boiling point) for 6 hours. As this result, the N-oxide disappeared, thus Process (c) being completed. Thereafter, pH of the reaction liquor was made to 8 with 62% sulfuric acid 19.0 g to precipitate a crystal. The precipitated crystal was separated by filtration, and the separated crystal was fully washed with water and further with methanol. The washed crystal was then dried, thus obtaining 11.6 g of 2-(2'-hydroxy-5'-t-butylphenyl)benzotriazole.

후처리

  1. customthus obtained
  2. temperaturethe liquor was heated to 55°~60° C
  3. customto precipitate a crystal
  4. customThe precipitated crystal was separated by filtration
  5. washthe separated crystal was fully washed with water and further with methanol
  6. customThe washed crystal was then dried

출처 및 근거

ORD 기록
ord-3effd731557643d5ad8e4a40f09dab5c
출처 데이터셋
uspto-grants-1989_05
특허 번호
US04835284

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