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

HRID 1664176ノート

反応式

HRID 1664176 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-8634b664e8e3422e91f71b2dfc71069d
出典データセット
uspto-grants-2011_10
特許番号
US08039458B2

反応ノート

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