Ethanol → 3-Chloro-5-(4-methyl-piperazin-1-yl)-benzoic acid

HRID 1946256ノート

反応式

HRID 1946256 の反応式
[Cl:1][C:2]1[CH:3]=C([CH:7]=[C:8]([N:10]2[CH2:15][CH2:14][N:13]([CH3:16])[CH2:12][CH2:11]2)[CH:9]=1)C#N.[OH-:17].[Na+].[CH2:19]([OH:21])[CH3:20]>Cl>[Cl:1][C:2]1[CH:3]=[C:20]([CH:7]=[C:8]([N:10]2[CH2:15][CH2:14][N:13]([CH3:16])[CH2:12][CH2:11]2)[CH:9]=1)[C:19]([OH:17])=[O:21]

参加物

5

反応物 3

HCID 702EthanolHCID 14798Sodium HydroxideHCID 591389873-Chloro-5-(4-methyl-piperazin-1-yl)-benzonitrile

生成物 1

HCID 591390453-Chloro-5-(4-methyl-piperazin-1-yl)-benzoic acid

試薬・触媒・溶媒 1

HCID 313Hydrochloric Acid溶媒

実験手順

To 3-chloro-5-(4-methyl-piperazin-1-yl)-benzonitrile (1.4 g, 5.9 mmol) dissolved in ethanol (10 ml) was added 2M NaOH (20 ml) and reaction mixture was heated at reflux for 20 hours. The mixture was reduced in vacuo and the crude product was acidified in 1N HCl to pH 6 and partitioned between EtOAc and H2O. The organic layer was evaporated to dryness in vacuo to give 0.7 g of the title compound as a white solid (LC/MS: Rt 1.67, [M+H]+ 256, acidic method).

後処理

  1. additionwas added
  2. temperaturewas heated
  3. temperatureat reflux for 20 hours
  4. custompartitioned between EtOAc and H2O
  5. customThe organic layer was evaporated to dryness in vacuo

出典と根拠

ORDレコード
ord-98c88d4299be47f993e5e71809f7e745
出典データセット
uspto-grants-2013_03
特許番号
US08399442B2

反応ノート

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