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

HRID 1946256노트

반응식

HRID 1946256 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 313Hydrochloric Acid용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-98c88d4299be47f993e5e71809f7e745
출처 데이터셋
uspto-grants-2013_03
특허 번호
US08399442B2

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