Citric Acid → 1-Methyl-1H-benzimidazole-5-carboxylic acid

HRID 1498913

반응식

HRID 1498913 반응식
[CH3:1][N:2]1[C:6]2[CH:7]=[CH:8][C:9]([C:11]([O:13]CC)=[O:12])=[CH:10][C:5]=2[N:4]=[CH:3]1.[OH-].[Na+].Cl.C(O)(=O)CC(CC(O)=O)(C(O)=O)O>CC(O)C>[CH3:1][N:2]1[C:6]2[CH:7]=[CH:8][C:9]([C:11]([OH:13])=[O:12])=[CH:10][C:5]=2[N:4]=[CH:3]1

참가 물질

6

반응물 4

HCID 311Citric AcidHCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 965320Ethyl 1-methyl-1h-benzimidazole-5-carboxylate

생성물 1

HCID 49130631-Methyl-1H-benzimidazole-5-carboxylic acid수율 86.2%

시약·촉매·용매 1

HCID 3776Isopropanol용매

실험 절차

Ethyl 1-methyl-1H-benzimidazole-5-carboxylate (800 mg, 3.92 mmol) prepared in the Step 1-1-4 was suspended in 2-propanol (10 ml), and a 1 mol/L sodium hydroxide aqueous solution (10 ml) was added thereto. The mixture was heated under reflux for one hour. After being allowed to cool, the mixture was neutralized with 1 mol/L hydrochloric acid. The resulting mixture was then acidified with citric acid, separated by filtration, and washed with a small quantity of water. Then, the resulting product was subjected to through circulation drying overnight to give the title compound (595 mg, 86%) as a gray powder.

후처리

  1. temperatureThe mixture was heated
  2. temperatureunder reflux for one hour
  3. temperatureto cool
  4. customseparated by filtration
  5. washwashed with a small quantity of water
  6. customdrying overnight

출처 및 근거

ORD 기록
ord-919dfc4e6f544d878b2785e4332178c9
출처 데이터셋
uspto-grants-2015_12
특허 번호
US09200008B2

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