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

HRID 1763177

反応式

HRID 1763177 の反応式
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

参加物

6

反応物 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

生成物 1

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

試薬・触媒・溶媒 1

HCID 10241Fluorenone触媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-3effd731557643d5ad8e4a40f09dab5c
出典データセット
uspto-grants-1989_05
特許番号
US04835284

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