1-(3,4-Dichlorophenyl)-1H-imidazole-4-carboxylic acid → HCID 23444980、化合物

HRID 433578ノート

反応式

HRID 433578 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([N:9]2[CH:13]=[C:12]([C:14](O)=[O:15])[N:11]=[CH:10]2)[CH:5]=[CH:6][C:7]=1[Cl:8]>CO>[Cl:1][C:2]1[CH:3]=[C:4]([N:9]2[CH:13]=[C:12]([CH2:14][OH:15])[N:11]=[CH:10]2)[CH:5]=[CH:6][C:7]=1[Cl:8]

参加物

3

反応物 1

HCID 234450601-(3,4-Dichlorophenyl)-1H-imidazole-4-carboxylic acid

生成物 1

HCID 23444980HCID 23444980、化合物

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
5 °C

実験手順

1-(3,4-Dichloro-phenyl)-1H-imidazole-4-carboxylic acid (20.0 g, 77.8 mmol) was treated with 1M BH3 THF complex (100 ml) and refluxed for 2 h. The mixture was cooled to 5° C. and MeOH (20 ml) was added slowly. After evaporation of all volatiles the residue was taken up in 2N HCl solution (100 ml) and refluxed for 2 h. After filtration the hot aqueous phase was slowly treated with 2N NaOH solution until pH 10. On cooling the title compound crystallizes as a white material (12.2 g, 65%). Mp. 146-147° C. (H2O), MS: m/e=242 (M+).

後処理

  1. temperaturerefluxed for 2 h
  2. customAfter evaporation of all volatiles the residue
  3. temperaturerefluxed for 2 h
  4. filtrationAfter filtration the hot aqueous phase
  5. additionwas slowly treated with 2N NaOH solution until pH 10
  6. temperatureOn cooling the title compound
  7. customcrystallizes as a white material (12.2 g, 65%)

出典と根拠

ORDレコード
ord-3fd3da5ac90247e28dc7f58dfb98f399
出典データセット
uspto-grants-2003_12
特許番号
US06667335B2

反応ノート

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