2-Ethylbutyraldehyde → 2-(4-Chlorobenzyl)-2-ethylbutanal

HRID 258264ノート

反応式

HRID 258264 の反応式
[OH-].[Na+].[CH2:3]([CH:5]([CH2:8][CH3:9])[CH:6]=[O:7])[CH3:4].[Cl:10][C:11]1[CH:18]=[CH:17][C:14]([CH2:15]Cl)=[CH:13][CH:12]=1>[I-].C([N+](CCCC)(CCCC)CCCC)CCC.C1(C)C=CC=CC=1>[Cl:10][C:11]1[CH:18]=[CH:17][C:14]([CH2:15][C:5]([CH2:8][CH3:9])([CH2:3][CH3:4])[CH:6]=[O:7])=[CH:13][CH:12]=1

参加物

6

反応物 3

HCID 73592-EthylbutyraldehydeHCID 77231-Chloro-4-(chloromethyl)benzeneHCID 14798Sodium Hydroxide

生成物 1

HCID 151008312-(4-Chlorobenzyl)-2-ethylbutanal

試薬・触媒・溶媒 2

HCID 67553Tetrabutylammonium Iodide触媒HCID 1140Toluene溶媒2 回

実験手順

300 ml of toluene, 400 ml of 30 percent (by weight) sodium hydroxide solution and 5.0 g of tetra-n-butyl-ammonium iodide are heated at 80° C. while stirring. To this is slowly added dropwise a mixture of 110 g (1.10 mol) of 2-ethylbutanal and 161 g (1.00 mol) of 4-chlorobenzyl chloride. The mixture is then stirred at 80° C. for 4 h and at room temperature for 14 h, 1,000 ml of toluene are added, and the phases are separated. The organic phase is washed with water, dried over Na2SO4 and concentrated. Fractional distillation results in 123 g (54% of theory) of 2-(4-chlorobenzyl) -2-ethylbutanal as a colorless liquid of boiling point 146°-148° C. at 1 mbar.

後処理

  1. additionTo this is slowly added dropwise
  2. stirringThe mixture is then stirred at 80° C. for 4 h and at room temperature for 14 h
  3. customthe phases are separated
  4. washThe organic phase is washed with water
  5. dry with materialdried over Na2SO4
  6. concentrationconcentrated
  7. distillationFractional distillation
  8. customresults in 123 g (54% of theory) of 2-(4-chlorobenzyl) -2-ethylbutanal as a colorless liquid of boiling point 146°-148° C. at 1 mbar

出典と根拠

ORDレコード
ord-b9ac554c1e4446a69a6e51b89084bc63
出典データセット
uspto-grants-1993_11
特許番号
US05266579

反応ノート

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