Toluene → 2-(2'-Hydroxy-3'5-di-tert-butylphenyl) benzotriazole

HRID 2082168

반응식

HRID 2082168 반응식
[N+:1]([C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=1[N:10]=[N:11][C:12]1[CH:17]=[C:16]([C:18]([CH3:21])([CH3:20])[CH3:19])[CH:15]=[C:14]([C:22]([CH3:25])([CH3:24])[CH3:23])[C:13]=1[OH:26])([O-])=O.C1(C)C=CC=CC=1.[OH-].[Na+].[H][H]>[C].[Pd].O.CC(O)C>[OH:26][C:13]1[C:14]([C:22]([CH3:25])([CH3:24])[CH3:23])=[CH:15][C:16]([C:18]([CH3:21])([CH3:20])[CH3:19])=[CH:17][C:12]=1[N:11]1[N:10]=[C:5]2[CH:6]=[CH:7][CH:8]=[CH:9][C:4]2=[N:1]1

참가 물질

8

반응물 4

HCID 1140TolueneHCID 14798Sodium HydroxideHCID 1041102,4-Bis(1,1-dimethylethyl)-6-[2-(2-nitrophenyl)diazenyl]phenolHCID 178418361HCID 178418361, 화합물2회

생성물 1

HCID 774552-(2'-Hydroxy-3'5-di-tert-butylphenyl) benzotriazole수율 73%

시약·촉매·용매 3

HCID 178418390HCID 178418390, 화합물촉매HCID 962Water용매HCID 3776Isopropanol용매

실험 절차

35.5 g (0.1 mol) of 2-nitro-2'-hydroxy-3',5'-di-t-butylazobenzene, 0.125 g of 5% palladium carbon, 100 ml of toluene, 100 ml of IPA, 100 ml water and 8.3 g of caustic soda were charged into a 500-ml stainless autoclave equipped with an agitator. After the air in the autoclave had been replaced by hydrogen, the pressure of hydrogen was set to 10 kg/cm2. Reaction was effected in the same way as that employed in Example 1. After the reaction had been completed, the catalyst was filtered off. When part of the filtrate was subjected to quantitative analysis using GC, it was found that the yield of 2-(2'-hydroxy-3',5'-di-t-butylphenyl)benzotriazole is 82%. After the solvent had been distilled off from the filtrate, the residual solid was crystallized by IPA, washed with IPA and then dried to obtain 23.6 g of 2-(2'-hydroxy-3',5'-di-t-butylphenyl)benzotriazole (yield, 73%; melting point, 150° to 152° C.).

후처리

  1. customequipped with an agitator
  2. customReaction
  3. filtrationthe catalyst was filtered off
  4. distillationAfter the solvent had been distilled off from the filtrate
  5. customthe residual solid was crystallized by IPA
  6. washwashed with IPA
  7. customdried

출처 및 근거

ORD 기록
ord-3d47e57f955241b7acc60e70a49c1ad4
출처 데이터셋
uspto-grants-1993_02
특허 번호
US05187289

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