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Bromine → 2-Methylbutyloxy-3-bromo-4-hydroxybiphenyl

HRID 648875
ノート
印刷プレビュー

反応式

HRID 648875 の反応式
[CH3:1][CH:2]([CH2:18][CH3:19])[CH2:3][O:4]C1C=CC(C2C=CC(O)=CC=2)=CC=1.CC(CC)CO[C:24]1[CH:29]=[CH:28][C:27]([C:30]2[CH:35]=[CH:34][C:33]([OH:36])=[C:32]([Br:37])[CH:31]=2)=[CH:26][CH:25]=1.BrBr>O1CCOCC1>[CH3:1][CH:2]([CH2:18][CH3:19])[CH2:3][O:4][C:31]1[C:32]([Br:37])=[C:33]([OH:36])[CH:34]=[CH:35][C:30]=1[C:27]1[CH:26]=[CH:25][CH:24]=[CH:29][CH:28]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 24408BromineHCID 140938154'-(2-Methylbutoxy)(1,1'-biphenyl)-4-olHCID 201439964'-(2-Methylbutyloxy)-3-bromo-4-hydroxybiphenyl

生成物 1

HCID 1317154892-Methylbutyloxy-3-bromo-4-hydroxybiphenyl

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒2 回

反応条件

温度
40 °C

実験手順

4'-(2-Methylbutyloxy)-4-hydroxybiphenyl (15 g) obtained in Example 1, (i) was dissolved in 1,4-dioxane (50 ml), followed by dropwise adding a mixture of bromine (10.5 g) and 1,4-dioxane (140 ml), heating on a water bath at 40° C. for 4 hours with stirring, thereafter distilling off 1,4-dioxane under reduced pressure, adding toluene (300 ml) to the remaining solution, adding a 10% aqueous solution of sodium hydrogen sulfite till the color of bromine disappeared, three times washing with saturated aqueous solution of NaCl to make the liquid neutral, drying and distilling off toluene to obtain a raw product of 4'-(2-methylbutyloxy-3-bromo-4-hydroxybiphenyl (21 g).

後処理

  1. additionby dropwise adding
  2. distillationdistilling off 1,4-dioxane under reduced pressure
  3. additionadding toluene (300 ml) to the remaining solution
  4. additionadding a 10% aqueous solution of sodium hydrogen sulfite till the color of bromine
  5. washthree times washing with saturated aqueous solution of NaCl
  6. customdrying
  7. distillationdistilling off toluene

出典と根拠

ORDレコード
ord-57b4796159e94c02a4489197e9942eae
出典データセット
uspto-grants-1988_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04737313

反応ノート

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