Potassium Hydroxide → 5-(4-chlorophenyl)-1-(2,4-dichlorophenyl)-1H-1,2,4-triazole-3-carboxylic acid

HRID 2251710ノート

反応式

HRID 2251710 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[N:12]([C:13]3[CH:18]=[CH:17][C:16]([Cl:19])=[CH:15][C:14]=3[Cl:20])[N:11]=[C:10]([C:21]([O:23]C)=[O:22])[N:9]=2)=[CH:4][CH:3]=1.[OH-].[K+]>CO>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[N:12]([C:13]3[CH:18]=[CH:17][C:16]([Cl:19])=[CH:15][C:14]=3[Cl:20])[N:11]=[C:10]([C:21]([OH:23])=[O:22])[N:9]=2)=[CH:4][CH:3]=1

参加物

4

反応物 2

HCID 14797Potassium HydroxideHCID 11246046methyl 5-(4-chlorophenyl)-1-(2,4-dichlorophenyl)-1H-1,2,4-triazole-3-carboxylate

生成物 1

HCID 111528615-(4-chlorophenyl)-1-(2,4-dichlorophenyl)-1H-1,2,4-triazole-3-carboxylic acid収率 92%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

Part C: To a stirred suspension of methyl 5-(4-chlorophenyl)-1-(2,4-dichlorophenyl)-1H-1,2,4-triazole-3-carboxylate (11.3 gram, 0.0295 mol) in methanol (100 mL) is added KOH (45% aqueous solution, 7.5 mL) and the resulting mixture is heated at reflux temperature for 4 hours. The mixture is concentrated in vacuo and water (150 mL) and concentrated HCl are added. The yellow precipitate is collected by filtration, washed with water and dried in vacuo to give 5-(4-chlorophenyl)-1-(2,4-dichlorophenyl)-1H-1,2,4-triazole-3-carboxylic acid (10.0 gram, 92% yield). Melting point: 141-144° C. (decomposition).

後処理

  1. temperaturethe resulting mixture is heated
  2. temperatureat reflux temperature for 4 hours
  3. concentrationThe mixture is concentrated in vacuo and water (150 mL) and concentrated HCl
  4. additionare added
  5. filtrationThe yellow precipitate is collected by filtration
  6. washwashed with water
  7. customdried in vacuo

出典と根拠

ORDレコード
ord-c8245ddd97be43319f2e95c709d51e5a
出典データセット
uspto-grants-2008_01
特許番号
US07319110B2

反応ノート

読み込み中…