Dimethylamine → Tinuvin

HRID 1030319

반응식

HRID 1030319 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.C1(C)C=CC=CC=1.CNC.[H][H]>[C].[Pd].O.C(O)CCC>[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

8

반응물 4

HCID 674DimethylamineHCID 1140TolueneHCID 141494702-(2-hydroxy-3-t-butyl-5-methylphenyl)-5-chlorobenzotriazole-N-oxideHCID 178418361HCID 178418361, 화합물3회

생성물 1

HCID 62531Tinuvin수율 86.1%

시약·촉매·용매 3

HCID 178418390HCID 178418390, 화합물촉매HCID 2631-Butanol용매HCID 962Water용매

실험 절차

33.2 g (0.1 mol) of 2-(2'-hydroxy-3'-t-butyl-5'-methylphenyl)-5-chlorobenzotriazole-N-oxide, 0.125 g of palladium carbon, 300 ml of a solvent mixture comprising toluene, butanol and water (ratio by volume of 1:1:1) and 5 g 50% dimethylamine 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 After the air in the autoclave had been replaced by hydrogen, the pressure of hydrogen was set to 10 kg/cm2. The temperature of the resultant mixture was increased to 50° C. under agitation, and agitation was continued until no more hydrogen gas was absorbed by the mixture. The pressure of hydrogen was always kept at 8 to 10 kg/cm2 during the reaction. After the reaction had been completed, the autoclave was cooled, and the catalyst was filtered off. The most part of solvent was distilled off, and the residual solid was washed with isopropyl alcohol and then dried to obtain 27.2 g of 2-(2'-hydroxy-3'-t-butyl- 5'-methylphenyl)-5-chlorobenzotriazole as a target substance (yield, 86.2%; melting point, 138° to 140° C.).

후처리

  1. additionwere charged into a 500-ml stainless autoclave
  2. customequipped with an agitator
  3. customwas absorbed by the mixture
  4. customThe pressure of hydrogen was always kept at 8 to 10 kg/cm2 during the reaction
  5. temperaturethe autoclave was cooled
  6. filtrationthe catalyst was filtered off
  7. distillationThe most part of solvent was distilled off
  8. washthe residual solid was washed with isopropyl alcohol
  9. customdried

출처 및 근거

ORD 기록
ord-24723d7b1a7641828cb4c0fff5e4aed4
출처 데이터셋
uspto-grants-1992_04
특허 번호
US05104992

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