3,4-Dichloroaniline → N-(3,4-dichlorophenyl)-4-pyridinecarboxamide-1-oxide

HRID 568403노트

반응식

HRID 568403 반응식
[N+:1]1([O-:10])[CH:6]=[CH:5][C:4]([C:7]([OH:9])=O)=[CH:3][CH:2]=1.C(N1C=CN=C1)(N1C=CN=C1)=O.[Cl:23][C:24]1[CH:25]=[C:26]([NH2:31])[CH:27]=[CH:28][C:29]=1[Cl:30]>CN(C)C=O>[Cl:23][C:24]1[CH:25]=[C:26]([NH:31][C:7]([C:4]2[CH:3]=[CH:2][N+:1]([O-:10])=[CH:6][CH:5]=2)=[O:9])[CH:27]=[CH:28][C:29]=1[Cl:30]

참가 물질

5

반응물 3

HCID 72573,4-DichloroanilineHCID 261304-Pyridinecarboxylic acid, 1-oxideHCID 682631,1'-Carbonyldiimidazole

생성물 1

HCID 13604807N-(3,4-dichlorophenyl)-4-pyridinecarboxamide-1-oxide수율 70.6%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

A suspension of 4-pyridinecarboxylic acid-1-oxide (3.74 g, 26.9 mmol) and 1,1'-Carbonyldiimidazole (4.80 g, 29.6 mmol) in dry dimethylformamide (50 ml) was stirred for 40 minutes under an air-lock and treated with 3,4-dichlorobenzenamine (4.79 g, 29.6 mmol). The reaction mixture was heated at 100° for 5.3 hours and cooled to room temperature. The solution was evaporated in vacuo and the residue triturated with ethanol (80 ml) to give the title compound (5.38 g), m.p. 259°-265°.

후처리

  1. temperatureThe reaction mixture was heated at 100° for 5.3 hours
  2. customThe solution was evaporated in vacuo
  3. customthe residue triturated with ethanol (80 ml)

출처 및 근거

ORD 기록
ord-ecabbf4affea4746a3a48b865638e7b7
출처 데이터셋
uspto-grants-1988_03
특허 번호
US04728658

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