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

HRID 258264노트

반응식

HRID 258264 반응식
[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

참가 물질

6

반응물 3

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

생성물 1

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

시약·촉매·용매 2

HCID 67553Tetrabutylammonium Iodide촉매HCID 1140Toluene용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-b9ac554c1e4446a69a6e51b89084bc63
출처 데이터셋
uspto-grants-1993_11
특허 번호
US05266579

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