Sulfuric Acid → (2-Methylbutyl)benzene

HRID 1086968ノート

反応式

HRID 1086968 の反応式
[C:1]1([Mg]Br)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.Br[C:10]1[CH:15]=[CH:14][CH:13]=CC=1.[Mg].OS(O)(=O)=O.[CH3:22]COCC>>[CH3:13][CH:14]([CH2:15][CH3:10])[CH2:22][C:1]1[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1

参加物

6

反応条件

温度
5 °C

実験手順

A phenylmagnesium bromide solution repapred from 40 g of bromobenzene, 6.2 g of magnesium and 300 ml of ether was cooled at 5° C., and a mixture liquid of 125 g of 2'-methylbutyl 4-methylbenzenesulfonate (II) prepared above and 130 ml of ether was added dropwise. After 2 hours of stirring, the mixture was elevated in temperature to effect 2 hours of refluxing, followed by standing overnight. To the reaction liquid, 10 % H2SO4 was added with pH 2. The organic layer was washed successively with an aqueous sodium bicarbonate solution and water, followed by drying with anhydrous magnesium sulfate, and distilling-off of the solvent. The product was distilled under reduced pressure to obtain 48 g of 4-(2'-methylbutyl)benzene (III) which showed the following IR data:

後処理

  1. additionwas added dropwise
  2. waitto effect 2 hours
  3. temperatureof refluxing
  4. waitby standing overnight
  5. additionwas added with pH 2
  6. washThe organic layer was washed successively with an aqueous sodium bicarbonate solution and water
  7. dry with materialby drying with anhydrous magnesium sulfate
  8. distillationThe product was distilled under reduced pressure

出典と根拠

ORDレコード
ord-eb9d62af387c4bb59fc2ddd4ed6edb2f
出典データセット
uspto-grants-1991_07
特許番号
US05034152

反応ノート

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