Acetic Acid → 3-Formylbut-2-enyl acetate

HRID 21848

반응식

HRID 21848 반응식
[C:1]1([CH3:7])[CH:6]=[CH:5]C=C[CH:2]=1.[C:8]([OH:11])(=[O:10])[CH3:9].[OH2:12]>>[C:8]([O:11][CH2:5][CH:6]=[C:1]([CH3:7])[CH:2]=[O:12])(=[O:10])[CH3:9]

참가 물질

4

반응물 3

HCID 176Acetic AcidHCID 962WaterHCID 1140Toluene

생성물 1

HCID 846993-Formylbut-2-enyl acetate수율 74%

반응 조건

온도
75 °C

실험 절차

4-Acetoxy-2-methyl-1-chloro-2-butene (7.8 g) was added to a suspension of hexamethylenetetramine (6.7 g) in acetonitrile (47 ml), and the mixture was stirred at room temperature for 16 hours. The resulting crystals were separated by filtration to give crystals (12.5 g) of the quaternary ammonium salt. The salt (7.9 g) was dissolved in water (50 ml), and toluene (100 ml) was added. Acetic acid (1.5 g per addition) was added 30 minutes, 1 hour and 2 hours after the beginning of the reaction with stirring at 75° C. The reaction was stopped 6 hours after the beginning of the reaction. The toluene layer was separated and concentrated. The remaining oil was purified by silica gel column chromatography to give 4-acetoxy-2-methyl-2-buten-1-al (2.6 g, 74%).

후처리

  1. customafter the beginning of the reaction
  2. customafter the beginning of the reaction
  3. customThe toluene layer was separated
  4. concentrationconcentrated
  5. customThe remaining oil was purified by silica gel column chromatography

출처 및 근거

ORD 기록
ord-d554762e6a2f46829719a1c5b6aee6ba
출처 데이터셋
uspto-grants-1995_06
특허 번호
US05424478

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