Acrylic Acid → 3-[(alpha-Methyl-4-chlorobenzylidene amino)oxy] propionic acid

HRID 2049035

반응식

HRID 2049035 반응식
[OH-].[Na+].[Cl:3][C:4]1[CH:9]=[CH:8][C:7]([C:10](=[N:12][OH:13])[CH3:11])=[CH:6][CH:5]=1.[C:14]([OH:18])(=[O:17])[CH:15]=[CH2:16]>C(O)C.O>[CH3:11][C:10](=[N:12][O:13][CH2:16][CH2:15][C:14]([OH:18])=[O:17])[C:7]1[CH:6]=[CH:5][C:4]([Cl:3])=[CH:9][CH:8]=1

참가 물질

6

반응물 3

HCID 6581Acrylic AcidHCID 14798Sodium HydroxideHCID 96172p-Chloroacetophenone oxime

생성물 1

HCID 544640573-[(alpha-Methyl-4-chlorobenzylidene amino)oxy] propionic acid

시약·촉매·용매 2

HCID 702Ethanol용매HCID 962Water용매

실험 절차

A solution of 2.4 g of sodium hydroxide in 55 ml of 85% ethanol was mixed with 6,78 g of 4'-chloroacetophenone oxime and 2.88 g of acrylic acid. The mixture was then refluxed for 2.5 hours, subsequently diluted with 10 ml of water, and concentrated by evaporation in a vacuum after 2 hours. The residue was dissolved in 50 ml of ether and 50 ml of water, and the layers were separated. The water layer was extracted with 50 ml of ether and then acidified with 40 ml of 2 N hydrochloric acid. The acid solution was extracted with 100 ml of ether and the ethereal solution was dried over sodium sulfate. Then the solvent was distilled off and its last traces were removed together with higher boiling substances at a pressure of 0.01 mm and a temperature of 50° C. The residue was crystallized from petroleum ether. Melting point 80° C.-83° C.

후처리

  1. temperatureThe mixture was then refluxed for 2.5 hours
  2. concentrationconcentrated by evaporation in a vacuum after 2 hours
  3. dissolutionThe residue was dissolved in 50 ml of ether
  4. custom50 ml of water, and the layers were separated
  5. extractionThe water layer was extracted with 50 ml of ether
  6. extractionThe acid solution was extracted with 100 ml of ether
  7. dry with materialthe ethereal solution was dried over sodium sulfate
  8. distillationThen the solvent was distilled off
  9. customits last traces were removed together with higher boiling substances at a pressure of 0.01 mm
  10. customa temperature of 50° C
  11. customThe residue was crystallized from petroleum ether

출처 및 근거

ORD 기록
ord-7b876a5a10b94343af915cc4c246854b
출처 데이터셋
uspto-grants-1980_04
특허 번호
US04196216

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