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Dichlone → 2-(2-hydroxy-3-t-butyl-5-methylphenyl)-5-chlorobenzotriazole-N-oxide

HRID 1763170
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HRID 1763170 반응식
[OH-].[Na+].[N+:3]([C:6]1[CH:11]=[C:10]([Cl:12])[CH:9]=[CH:8][C:7]=1[N:13]=[N:14][C:15]1[CH:20]=[C:19]([CH3:21])[CH:18]=[C:17]([C:22]([CH3:25])([CH3:24])[CH3:23])[C:16]=1[OH:26])([O-])=O.ClC1C(=O)C2C(C(=[O:39])C=1Cl)=CC=CC=2.O=C[C@@H]([C@H]([C@@H]([C@@H](CO)O)O)O)O>CO>[OH:26][C:16]1[C:17]([C:22]([CH3:25])([CH3:24])[CH3:23])=[CH:18][C:19]([CH3:21])=[CH:20][C:15]=1[N:14]1[N+:13]([O-:39])=[C:7]2[CH:8]=[CH:9][C:10]([Cl:12])=[CH:11][C:6]2=[N:3]1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

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HCID 8342DichloneHCID 14798Sodium HydroxideHCID 89771Phenol, 2-[2-(4-chloro-2-nitrophenyl)diazenyl]-6-(1,1-dimethylethyl)-4-methyl-HCID 107526(2R,3S,4R,5R)-2,3,4,5,6-pentahydroxyhexanal

생성물 1

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

시약·촉매·용매 1

HCID 887
Methanol
용매

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온도
65 °C

실험 절차

97% sodium hydroxide 9.6 g was added to methanol 100 ml, and was stirred at 65° C. for 30 minutes. After cooling to 50° C., 2-nitro-4-chloro-2'-hydroxy-3'-t-butyl-5'-methylazobenzene 11.6 g was added to the resultant mixture over 30 minutes, and thereafter 2,3-dichloro-1,4-naphthoquinone 0.7 g was added. Glucose 8 g was added to the resultant mixture at 40° to 45° C. over one hour, and the mixture was stirred for one hour at 40° to 45° C. As this result, almost all of the azobenzenes disappeared to produce 2-(2'-hydroxy-3'-t-butyl-5'-methylphenyl)-5-chlorobenzotriazole-N-oxide, thus the reaction of Process (b) being completed.

후처리

  1. temperatureAfter cooling to 50° C.
  2. stirringthe mixture was stirred for one hour at 40° to 45° C

출처 및 근거

ORD 기록
ord-3a240b3f143a45b2ab420563fe6ede0e
출처 데이터셋
uspto-grants-1989_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04835284

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