Sulfuric Acid → Tinuvin

HRID 1763173

반응식

HRID 1763173 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

HCID 62531Tinuvin수율 82.9%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

In order to conduct the reaction of Process (c), the system was heated, and was stirred at 66° to 68° C. (boiling point) for 5 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 10 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 8.7 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 82.9%.

후처리

  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

출처 및 근거

ORD 기록
ord-b87118cb457540f9b227a12747cf0e34
출처 데이터셋
uspto-grants-1989_05
특허 번호
US04835284

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