Hydrochloric Acid → 2-(2-(2-Bromo-5-fluorophenyl)hydrazono)acetic acid

HRID 1664176노트

반응식

HRID 1664176 반응식
[Br:1][C:2]1[CH:7]=[CH:6][C:5]([F:8])=[CH:4][C:3]=1[NH:9][NH2:10].Cl.O.[C:13]([OH:17])(=[O:16])[CH:14]=O>O>[Br:1][C:2]1[CH:7]=[CH:6][C:5]([F:8])=[CH:4][C:3]=1[NH:9][N:10]=[CH:14][C:13]([OH:17])=[O:16]

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 12891829(2-Bromo-5-fluorophenyl)hydrazineHCID 15620607Glyoxylic acid, monohydrate

생성물 1

HCID 674393932-(2-(2-Bromo-5-fluorophenyl)hydrazono)acetic acid수율 98%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

To a solution of (2-bromo-5-fluorophenyl)hydrazine (2.15 g, 10.5 mmol) and concentrated HCl (1.2 mL) in water (30 mL) was added glyoxylic acid hydrate (1.06 g, 11.5 mmol). The resulting mixture was stirred at room temperature for 2 h. The precipitate that formed was collected by filtration, washed with water and dried at reduced pressure to afford the title compound as a yellow solid (2.67 g, 98% yield): 1H NMR (400 MHz, DMSO-D6) δ ppm 12.57 (1H, s), 10.65 (1H, s), 7.65 (1H, s), 7.56 (1H, dd, J=8.7, 5.9 Hz), 7.31 (1H, dd, J=11.4, 3.0 Hz), 6.73 (1H, td, J=8.5, 3.0 Hz); LCMS (+ESI, M+H+) m/z 261-263.

후처리

  1. customThe precipitate that formed
  2. filtrationwas collected by filtration
  3. washwashed with water
  4. customdried at reduced pressure

출처 및 근거

ORD 기록
ord-8634b664e8e3422e91f71b2dfc71069d
출처 데이터셋
uspto-grants-2011_10
특허 번호
US08039458B2

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