Dibutyltin oxide → 2,2'-{(Dibutylstannylene)bis[oxy-(5-tert-octyl-2,l-phenylene)]}bis-(2H-benzotriazole)

HRID 433652

반응식

HRID 433652 반응식
[OH:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]([CH2:11][C:12]([CH3:15])([CH3:14])[CH3:13])([CH3:10])[CH3:9])=[CH:4][C:3]=1[N:16]1[N:20]=[C:19]2[CH:21]=[CH:22][CH:23]=[CH:24][C:18]2=[N:17]1.[CH2:25]([Sn:29](=[O:34])[CH2:30][CH2:31][CH2:32][CH3:33])[CH2:26][CH2:27][CH3:28]>C1(C)C=CC=CC=1>[CH2:25]([Sn:29]([CH2:30][CH2:31][CH2:32][CH3:33])([O:34][C:2]1[CH:7]=[CH:6][C:5]([C:8]([CH2:11][C:12]([CH3:13])([CH3:14])[CH3:15])([CH3:9])[CH3:10])=[CH:4][C:3]=1[N:16]1[N:17]=[C:18]2[CH:24]=[CH:23][CH:22]=[CH:21][C:19]2=[N:20]1)[O:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]([CH2:11][C:12]([CH3:13])([CH3:14])[CH3:15])([CH3:9])[CH3:10])=[CH:4][C:3]=1[N:16]1[N:20]=[C:19]2[CH:21]=[CH:22][CH:23]=[CH:24][C:18]2=[N:17]1)[CH2:26][CH2:27][CH3:28]

참가 물질

4

반응물 2

HCID 61221Dibutyltin oxideHCID 62485Octrizole

생성물 1

HCID 700158602,2'-{(Dibutylstannylene)bis[oxy-(5-tert-octyl-2,l-phenylene)]}bis-(2H-benzotriazole)수율 43.3%

시약·촉매·용매 1

HCID 1140Toluene용매

반응 조건

온도
2.5 °C

실험 절차

2-(2-Hydroxy-5-tert-octylphenyl)-2H-benzotriazole (64.6 g, 0.2 mol, TINUVIN® 329, CIBA), dibutyltin oxide (24.89 g, 0.1 mol) and toluene are charged to a laboratory reactor and the contents are heated to reflux and refluxed for seven hours. About half of the amount of toluene is removed by distillation. The reaction mass is cooled to 0-5° C. after the addition of 200 g of hexane. Any unreacted TINUVIN® 329 and dibutyltin oxide are removed by filtration. The solvent is then removed by distillation to yield the title compound (38 g, 43.3% yield) as a yellow resin whose structure is consistent with 1Hnmr analysis.

후처리

  1. temperaturethe contents are heated
  2. temperatureto reflux
  3. temperaturerefluxed for seven hours
  4. customAbout half of the amount of toluene is removed by distillation
  5. additionafter the addition of 200 g of hexane
  6. customAny unreacted TINUVIN® 329 and dibutyltin oxide are removed by filtration
  7. customThe solvent is then removed by distillation

출처 및 근거

ORD 기록
ord-4819dd734c184c8e900ec89be064cb1a
출처 데이터셋
uspto-grants-2003_12
특허 번호
US06667403B2

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