2-Fluorobenzoyl chloride → 2-Fluorobenzoic acid, 2-(4-(trifluoromethyl)phenyl)hydrazide

HRID 359020

반응식

HRID 359020 반응식
[F:1][C:2]([F:12])([F:11])[C:3]1[CH:8]=[CH:7][C:6]([NH:9][NH2:10])=[CH:5][CH:4]=1.[F:13][C:14]1[CH:22]=[CH:21][CH:20]=[CH:19][C:15]=1[C:16](Cl)=[O:17]>N1C=CC=CC=1>[F:1][C:2]([F:11])([F:12])[C:3]1[CH:4]=[CH:5][C:6]([NH:9][NH:10][C:16](=[O:17])[C:15]2[CH:19]=[CH:20][CH:21]=[CH:22][C:14]=2[F:13])=[CH:7][CH:8]=1

참가 물질

4

반응물 2

HCID 98082-Fluorobenzoyl chlorideHCID 1362004-(Trifluoromethyl)phenylhydrazine

생성물 1

HCID 151170472-Fluorobenzoic acid, 2-(4-(trifluoromethyl)phenyl)hydrazide수율 85%

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

To a stirred solution of 75.0 g of 4-(trifluoromethyl)-phenylhydrazine in 500 ml of dry pyridine, cooled in an ice bath, was added dropwise, under nitrogen, 79.1 g of 2-fluorobenzoyl chloride. Upon completion of the addition, the ice bath was removed and the reaction mixture stirred at ambient temperature for 4 hours. The mixture was poured into water and a precipitate formed. Recrystallization of the precipitate from isopropyl alcohol-water, gave 108 g (84%) of 2-fluorobenzoic acid, 2-(4-(trifluoromethyl)phenyl)hydrazide as a solid. Subsequent recrystallization from isopropyl alcohol-water gave the analytical sample, mp 163°-165°.

후처리

  1. additionwas added dropwise, under nitrogen
  2. additionUpon completion of the addition
  3. customthe ice bath was removed
  4. additionThe mixture was poured into water
  5. customa precipitate formed
  6. customRecrystallization of the precipitate from isopropyl alcohol-water

출처 및 근거

ORD 기록
ord-84092de639474d16a10f7b220f423f39
출처 데이터셋
uspto-grants-1991_03
특허 번호
US04999356

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