Sulfuric Acid → Tinuvin

HRID 1763171

反応式

HRID 1763171 の反応式
[OH:1][C:2]1[C:7]([C:8]([CH3:11])([CH3:10])[CH3:9])=[CH:6][C:5]([CH3:12])=[CH:4][C:3]=1[N:13]1[N+:17]([O-])=[C:16]2[CH:19]=[CH:20][C:21]([Cl:23])=[CH:22][C:15]2=[N:14]1.S(=O)(=O)(O)O>O>[OH:1][C:2]1[C:7]([C:8]([CH3:10])([CH3:9])[CH3:11])=[CH:6][C:5]([CH3:12])=[CH:4][C:3]=1[N:13]1[N:17]=[C:16]2[CH:19]=[CH:20][C:21]([Cl:23])=[CH:22][C:15]2=[N:14]1

参加物

4

反応物 2

HCID 1118Sulfuric AcidHCID 141494702-(2-hydroxy-3-t-butyl-5-methylphenyl)-5-chlorobenzotriazole-N-oxide

生成物 1

HCID 62531Tinuvin収率 89.5%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

In order to conduct the reaction of Process (c), the system was heated, and was stirred at 64° to 67° C. for two hours. As this result, the N-oxide disappeared, thus Process (c) being completed. Thereafter, water 50 ml was added to the reaction liquor, and the resultant reaction liquor was neutralized with 62% sulfuric acid 11 g to precipitate a crystal. The precipitated crystal was separated by filtration, and the separated crystal was fully washed with hot water of 60° to 70° C. and further with a small amount of methanol. The washed crystal was then dried, thus obtaining 9.4 g of 2-(2'-hydroxy-3'-t-butyl-5'-methylphenyl)-5-chlorobenzotriazole having a melting point of 138° to 140° C. at the yield of 89.5%.

後処理

  1. temperaturethe system was heated
  2. customthe resultant reaction liquor
  3. customto precipitate a crystal
  4. customThe precipitated crystal was separated by filtration
  5. washthe separated crystal was fully washed with hot water of 60° to 70° C. and further with a small amount of methanol
  6. customThe washed crystal was then dried

出典と根拠

ORDレコード
ord-e0385dc1bd0847e5a7a019ac48327eea
出典データセット
uspto-grants-1989_05
特許番号
US04835284

関連ノート

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