Potassium Carbonate → 2-(2-Fluorophenyl)-1-hydroxy-4-methyl-5-(3-pyridyl)imidazole

HRID 620839ノート

反応式

HRID 620839 の反応式
[OH:1][N:2]=[C:3]([C:7]1[CH:8]=[N:9][CH:10]=[CH:11][CH:12]=1)[C:4]([CH3:6])=O.[F:13][C:14]1[CH:21]=[CH:20][CH:19]=[CH:18][C:15]=1[CH:16]=O.C([O-])(=O)C.[NH4+:26].C(=O)([O-])[O-].[K+].[K+]>C(O)(=O)C.O>[F:13][C:14]1[CH:21]=[CH:20][CH:19]=[CH:18][C:15]=1[C:16]1[N:2]([OH:1])[C:3]([C:7]2[CH:8]=[N:9][CH:10]=[CH:11][CH:12]=2)=[C:4]([CH3:6])[N:26]=1

参加物

7

反応物 4

HCID 11430Potassium CarbonateHCID 67970o-FluorobenzaldehydeHCID 517165Ammonium AcetateHCID 737518861-Hydroxyimino-1-(3-pyridyl)acetone

生成物 1

HCID 103332812-(2-Fluorophenyl)-1-hydroxy-4-methyl-5-(3-pyridyl)imidazole収率 28%

試薬・触媒・溶媒 2

HCID 176Acetic Acid溶媒HCID 962Water溶媒

実験手順

To a solution 1-hydroxyimino-1-(3-pyridyl)acetone (0.5 g) in acetic acid (10 ml) was added 2-fluorobenzaldehyde (0.76 g) and ammonium acetate (2.35 g), and refluxed for 30 minutes. Then, the solution was poured into water (75 ml), neutrallized with aqueous potassium carbonate, and extracted with ethyl acetate. The extract was dried over magnesium sulfate and concentrated, and the residue was triturated with diisopropyl ether to give 2-(2-fluorophenyl)-1-hydroxy-4-methyl-5-(3-pyridyl)imidazole (0.23 g).

後処理

  1. temperaturerefluxed for 30 minutes
  2. extractionextracted with ethyl acetate
  3. dry with materialThe extract was dried over magnesium sulfate
  4. concentrationconcentrated
  5. customthe residue was triturated with diisopropyl ether

出典と根拠

ORDレコード
ord-70513545ded44daea38c5ae6eea9060e
出典データセット
uspto-grants-1989_04
特許番号
US04822805

反応ノート

読み込み中…