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

HRID 433652

反応式

HRID 433652 の反応式
[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]

参加物

4

反応物 2

HCID 61221Dibutyltin oxideHCID 62485Octrizole

生成物 1

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

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

反応条件

温度
2.5 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-4819dd734c184c8e900ec89be064cb1a
出典データセット
uspto-grants-2003_12
特許番号
US06667403B2

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