Hydrochloric Acid → 4-Bromo-5-fluoro-2-hydrazinylbenzoic acid hydrochloride

HRID 523234

반응식

HRID 523234 반응식
[Br:1][C:2]1[C:10]([F:11])=[CH:9][C:5]([C:6]([OH:8])=[O:7])=[C:4](F)[CH:3]=1.[NH2:13][NH2:14].[ClH:15]>CN1CCCC1=O>[ClH:15].[Br:1][C:2]1[C:10]([F:11])=[CH:9][C:5]([C:6]([OH:8])=[O:7])=[C:4]([NH:13][NH2:14])[CH:3]=1

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 9321HydrazineHCID 8228574-Bromo-2,5-difluorobenzoic acid

생성물 1

HCID 768481964-Bromo-5-fluoro-2-hydrazinylbenzoic acid hydrochloride수율 44%

시약·촉매·용매 1

HCID 13387N-methyl-2-pyrrolidone용매

반응 조건

온도
95 °C

실험 절차

A mixture of 4-bromo-2,5-difluorobenzoic acid (2.50 g, 10.6 mmol) and hydrazine (3.81 mL, 121 mmol) in N-methyl-2-pyrrolidinone (2 mL) was heated at 95° C. for 4 h. The cooled mixture was poured into vigorously stirred 6 M aqueous HCl (400 mL) which was cooled in an NaCl-ice bath. The resulting precipitate was collected by filtration, washed with 6 M aqueous HCl (200 mL) and dried under vacuum to give 4-bromo-5-fluoro-2-hydrazinylbenzoic acid hydrochloride as a yellow solid (1.88 g, 71% purity, 44% yield), used without further purification.

후처리

  1. temperaturewas cooled in an NaCl-ice bath
  2. filtrationThe resulting precipitate was collected by filtration
  3. washwashed with 6 M aqueous HCl (200 mL)
  4. customdried under vacuum

출처 및 근거

ORD 기록
ord-7d586237e60148f69ccfc0d9b881c500
출처 데이터셋
uspto-grants-2016_05
특허 번호
US09334290B2

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