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Hydrochloric Acid → N-(3,5-dichloro-2-pyridyl)-2,4-dinitro-6-trifluoromethylaniline

HRID 1065775
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HRID 1065775 반응식
[NH2:1][C:2]1[C:7]([Cl:8])=[CH:6][C:5]([Cl:9])=[CH:4][N:3]=1.[OH-].[K+].[N+:12]([C:15]1[CH:20]=[C:19]([N+:21]([O-:23])=[O:22])[CH:18]=[C:17]([C:24]([F:27])([F:26])[F:25])[C:16]=1Cl)([O-:14])=[O:13].Cl>CN(C)C=O>[Cl:8][C:7]1[C:2]([NH:1][C:16]2[C:17]([C:24]([F:26])([F:27])[F:25])=[CH:18][C:19]([N+:21]([O-:23])=[O:22])=[CH:20][C:15]=2[N+:12]([O-:14])=[O:13])=[N:3][CH:4]=[C:5]([Cl:9])[CH:6]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 14797Potassium HydroxideHCID 67851Benzene, 2-chloro-1,5-dinitro-3-(trifluoromethyl)-HCID 778863,5-Dichloro-3-pyridylamine

생성물 1

HCID 12901603N-(3,5-dichloro-2-pyridyl)-2,4-dinitro-6-trifluoromethylaniline

시약·촉매·용매 1

HCID 6228
Dimethylformamide
용매

실험 절차

In 20 ml. of dimethylformamide, 1.65 g. of 2-amino-3,5-dichloropyridine was dissolved and 1.0 g. of powdery potassium hydroxide was gradually added with stirring. After the addition, 2.7 g. of 2,4-dinitro-6-trifluoromethylchlorobenzene was added at 30° C. during 5 minutes to react them for about 3 hours. The reaction mixture was acidified with conc. HCl and the product was extracted with methylenechloride. The extracted layer was washed with water and dehydrated and the solvent was distilled. The product was separated by a silica gel column with an eluent of toluene and the solvent was distilled off to obtain 2.5 g. of the object compound having the melting point of 98° to 101° C.

후처리

  1. additionAfter the addition, 2.7 g
  2. customto react them for about 3 hours
  3. extractionthe product was extracted with methylenechloride
  4. washThe extracted layer was washed with water
  5. distillationthe solvent was distilled
  6. customThe product was separated by a silica gel column with an eluent of toluene
  7. distillationthe solvent was distilled off
  8. customto obtain 2.5 g

출처 및 근거

ORD 기록
ord-043b4204da8040d5ae03f1aa5352abee
출처 데이터셋
uspto-grants-1982_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04331670

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