Pyridine → 2',6'-Dinitro-4'-trifluoromethyl-2,2,2-trifluoroacetanilide

HRID 1576377

반응식

HRID 1576377 반응식
[N+:1]([C:4]1[CH:10]=[C:9]([C:11]([F:14])([F:13])[F:12])[CH:8]=[C:7]([N+:15]([O-:17])=[O:16])[C:5]=1[NH2:6])([O-:3])=[O:2].N1C=CC=CC=1.[F:24][C:25]([F:30])([F:29])[C:26](Cl)=[O:27].FC(F)(F)C(O)=O>C(O)C>[N+:1]([C:4]1[CH:10]=[C:9]([C:11]([F:12])([F:13])[F:14])[CH:8]=[C:7]([N+:15]([O-:17])=[O:16])[C:5]=1[NH:6][C:26](=[O:27])[C:25]([F:30])([F:29])[F:24])([O-:3])=[O:2]

참가 물질

6

반응물 4

HCID 1049PyridineHCID 6422Trifluoroacetic acidHCID 99362,6-Dinitro-4-(trifluoromethyl)anilineHCID 61106Trifluoroacetyl chloride

생성물 1

HCID 215124262',6'-Dinitro-4'-trifluoromethyl-2,2,2-trifluoroacetanilide

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A solution of 25.1 g. of 2,6-dinitro-4-trifluoromethylaniline in 100 ml. of pyridine was treated with trifluoroacetyl chloride, which has been prepared from 10 ml. of trifluoroacetic acid. Ethanol was added to the resulting mixture until it was homogeneous, and the reaction mixture was then evaporated under vacuum. The residue after evaporation was washed with water, dried, dissolved in acetone, and filtered. Chloroform was added to the filtrate until the product precipitated. The precipitate was separated by filtration and dried to obtain the purified intermediate, 2',6'-dinitro-4'-trifluoromethyl-2,2,2-trifluoroacetanilide.

후처리

  1. customhas been prepared from 10 ml
  2. customthe reaction mixture was then evaporated under vacuum
  3. customThe residue after evaporation
  4. washwas washed with water
  5. customdried
  6. dissolutiondissolved in acetone
  7. filtrationfiltered
  8. additionChloroform was added to the filtrate until the product
  9. customprecipitated
  10. customThe precipitate was separated by filtration
  11. customdried

출처 및 근거

ORD 기록
ord-2acf227a1cfb4dcdbbbcc2e56b5f5bcc
출처 데이터셋
uspto-grants-1976_09
특허 번호
US03980784

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