Toluene → 2,4-Di-tert-butyl-6-(5-chloro-2H-benzotriazol-2-yl)phenol

HRID 1030318ノート

反応式

HRID 1030318 の反応式
[OH:1][C:2]1[C:7]([C:8]([CH3:11])([CH3:10])[CH3:9])=[CH:6][C:5]([C:12]([CH3:15])([CH3:14])[CH3:13])=[CH:4][C:3]=1[N:16]1[N+:20]([O-])=[C:19]2[CH:22]=[CH:23][C:24]([Cl:26])=[CH:25][C:18]2=[N:17]1.C1(C)C=CC=CC=1.N12CCCCC1CNCC=C2.[H][H]>[Ni].CC(O)CC>[OH:1][C:2]1[C:7]([C:8]([CH3:10])([CH3:11])[CH3:9])=[CH:6][C:5]([C:12]([CH3:13])([CH3:14])[CH3:15])=[CH:4][C:3]=1[N:16]1[N:20]=[C:19]2[CH:22]=[CH:23][C:24]([Cl:26])=[CH:25][C:18]2=[N:17]1

参加物

7

反応物 4

HCID 1140TolueneHCID 141494712-(2-hydroxy-3,5-di-t-butylphenyl)-5-chlorobenzotriazole-N-oxideHCID 226720701,5-Diazabicyclo[5.4.0]undeceneHCID 178418361HCID 178418361、化合物2 回

生成物 1

HCID 774702,4-Di-tert-butyl-6-(5-chloro-2H-benzotriazol-2-yl)phenol収率 78.8%

試薬・触媒・溶媒 2

HCID 935Nickel触媒HCID 6568(+-)-2-Butanol溶媒

実験手順

37.4 g (0.1 mol) of 2-(2'-hydroxy-3',5'-di-t-butylphenyl)-5-chlorobenzotriazole-N-oxide, 0.25 g of Raney nickel catalyst, 150 ml of toluene, 100 ml of 2-butanol and 0.5 g of 1,5-diazabicyclo[5.4.0]undecene were charged into a 500-ml stainless autoclave equipped with an agitator. After the air in the autoclave had been replaced by nitrogen, hydrogen was charged to a pressure of 8 kg/cm2. The temperature of the resultant mixture was increased to 60° C. under agitation, and reaction was been effected while agitation being continued until no hydrogen gas was absorbed by the mixture. After the reaction had been completed, after treatment was performed in the same way as that employed in Example 9 to obtain 28.2 g of 2-(2'-hydroxy-3',5'-di-t-butylphenyl)-5-chlorobenzotriazole as a target substance (yield, 79%; melting point, 153° to 155° C.).

後処理

  1. customequipped with an agitator
  2. additionwas charged to a pressure of 8 kg/cm2
  3. customwas absorbed by the mixture

出典と根拠

ORDレコード
ord-0027f4a0cd2f44948f6ee117a6e69b2f
出典データセット
uspto-grants-1992_04
特許番号
US05104992

反応ノート

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