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Pyridine → 2,4-Dinitrophenylbenzamide

HRID 986818
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HRID 986818 반응식
[N+:1]([C:4]1[CH:10]=[C:9]([N+:11]([O-:13])=[O:12])[CH:8]=[CH:7][C:5]=1N)([O-:3])=[O:2].[C:14](Cl)(=[O:21])[C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1.[N:23]1C=CC=CC=1>>[N+:1]([C:4]1[CH:10]=[C:9]([N+:11]([O-:13])=[O:12])[CH:8]=[CH:7][C:5]=1[C:16]1[CH:17]=[CH:18][CH:19]=[CH:20][C:15]=1[C:14]([NH2:23])=[O:21])([O-:3])=[O:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 3

HCID 1049PyridineHCID 73212,4-DinitroanilineHCID 7412Benzoyl chloride

생성물 1

HCID 201563782,4-Dinitrophenylbenzamide

실험 절차

To a solution of 73.2 g. (0.4 m.) of 2,4-dinitroaniline in 400 ml. of pyridine with stirring and slight warming is added 56.2 g. (0.4 m.) of benzoyl chloride in about 10 min.; the temperature rises from 40° to 50°. Then the dark solution is heated at reflux for 21/2 hours. After standing overnight, the yellow solid is collected, washed with H2O until no pyridine odor is detectable. This 90 g. of crude product is recrystallized from about 2.1 of CH3CN to yield 44 g. (38%) of yellow product melting at 201°-205°.

후처리

  1. temperatureslight warming
  2. addition
is added 56.2 g
  • customrises from 40° to 50°
  • temperatureThen the dark solution is heated
  • temperatureat reflux for 21/2 hours
  • customthe yellow solid is collected
  • washwashed with H2O until no pyridine odor
  • customof crude product is recrystallized from about 2.1 of CH3CN
  • customto yield 44 g
  • 출처 및 근거

    ORD 기록
    ord-7da71810bee64d97941cc6ab73feae9f
    출처 데이터셋
    uspto-grants-1987_12
    DOI
    10.6084/m9.figshare.5104873.v1
    특허 번호
    US04716168

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