Hydrochloric Acid → 5-Amino-1-(2,3,5,6-tetrafluoro-4-trifluoromethylphenyl)-4-nitropyrazole

HRID 2232179노트

반응식

HRID 2232179 반응식
C([NH:4][C:5]1[N:9]([C:10]2[C:15]([F:16])=[C:14]([F:17])[C:13]([C:18]([F:21])([F:20])[F:19])=[C:12]([F:22])[C:11]=2[F:23])[N:8]=[CH:7][C:6]=1[N+:24]([O-:26])=[O:25])(=O)C.Cl.C(O)C.[OH-].[Na+]>O>[NH2:4][C:5]1[N:9]([C:10]2[C:15]([F:16])=[C:14]([F:17])[C:13]([C:18]([F:20])([F:21])[F:19])=[C:12]([F:22])[C:11]=2[F:23])[N:8]=[CH:7][C:6]=1[N+:24]([O-:26])=[O:25]

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 702Ethanol2회HCID 14798Sodium HydroxideHCID 139337121-(2,3,5,6-Tetrafluoro-4-trifluoromethyl phenyl)-5-methylcarbonylamino-4-nitropyrazole

생성물 1

HCID 139337135-Amino-1-(2,3,5,6-tetrafluoro-4-trifluoromethylphenyl)-4-nitropyrazole수율 91.4%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

19.3 g (0.05 mol) of 5-acetamido-4-nitro-1-(2,3,5,6-tetrafluoro-4-trifluoromethyl-phenyl)-pyrazole are heated under reflux in a mixture of 40 ml of 37 percent strength hydrochloric acid and 70 ml of ethanol for 7 hours. The reaction mixture is freed from the ethanol in vacuo. 35 ml of water are added to the residue and the mixture is neutralized with dilute sodium hydroxide solution. The precipitate is filtered off with suction, washed with water and dried in vacuo. 15.7 g (91.4% of theory) of 5-amino-4-nitro-1-(2,3,5,6-tetrafluoro-4-trifluoromethyl-phenyl)-pyrazole of melting point 123° C.-126° C. are obtained.

후처리

  1. filtrationThe precipitate is filtered off with suction
  2. washwashed with water
  3. customdried in vacuo

출처 및 근거

ORD 기록
ord-24b7690c4d3a421da3e961e4dcf7f517
출처 데이터셋
uspto-grants-1988_11
특허 번호
US04787930

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