3,4-Dimethoxy-2-nitrobenzaldehyde → 3,4-dimethoxy-2-nitrobenzoic acid

HRID 1577339노트

반응식

HRID 1577339 반응식
[Mn]([O-])(=O)(=O)=[O:2].[K+].[CH3:7][O:8][C:9]1[C:10]([N+:19]([O-:21])=[O:20])=[C:11]([CH:14]=[CH:15][C:16]=1[O:17][CH3:18])[CH:12]=[O:13]>O.CC(C)=O>[CH3:7][O:8][C:9]1[C:10]([N+:19]([O-:21])=[O:20])=[C:11]([CH:14]=[CH:15][C:16]=1[O:17][CH3:18])[C:12]([OH:2])=[O:13]

참가 물질

5

반응물 2

HCID 1524373,4-Dimethoxy-2-nitrobenzaldehydeHCID 516875Potassium Permanganate

생성물 1

HCID 12522693,4-dimethoxy-2-nitrobenzoic acid

시약·촉매·용매 2

HCID 180Acetone용매HCID 962Water용매

실험 절차

A solution of 823 g. potassium permanganate in about 8.5 liters of H2O was gradually added to a refluxing solution of 3,4-dimethoxy-2-nitrobenzaldehyde (550 g., 2.60 moles) in 5.6 liters of acetone. The reaction mixture was refluxed for four more hours, then filtered through diatomaceous earth while hot and the filter cake washed with hot water. The acetone was removed in vacuo and a small amount of unreacted solid was filtered off. The aqueous solution was acidified with 2 N hydrochloric acid (1.8 liters) to yield 505 g. (85% ) of the essentially pure title compound. Recrystallization from water afforded colorless crystals, M.P. 200°-202° C.

후처리

  1. temperatureThe reaction mixture was refluxed for four more hours
  2. filtrationfiltered through diatomaceous earth while hot and the filter cake
  3. washwashed with hot water
  4. customThe acetone was removed in vacuo
  5. filtrationa small amount of unreacted solid was filtered off
  6. customto yield 505 g

출처 및 근거

ORD 기록
ord-85e2a74132a3449985c5f45d75a2b947
출처 데이터셋
uspto-grants-1981_09
특허 번호
US04287341

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