Hydrochloric Acid → 1-Methyl-4-[({[4-(trifluoromethoxy)phenyl]amino}carbonyl)amino]-1H-imidazole-2-carboxylic Acid

HRID 2277416노트

반응식

HRID 2277416 반응식
C([O:3][C:4]([C:6]1[N:7]([CH3:26])[CH:8]=[C:9]([NH:11][C:12]([NH:14][C:15]2[CH:20]=[CH:19][C:18]([O:21][C:22]([F:25])([F:24])[F:23])=[CH:17][CH:16]=2)=[O:13])[N:10]=1)=[O:5])C.[OH-].[Na+].Cl>C(O)C.O1CCCC1>[CH3:26][N:7]1[CH:8]=[C:9]([NH:11][C:12]([NH:14][C:15]2[CH:20]=[CH:19][C:18]([O:21][C:22]([F:23])([F:25])[F:24])=[CH:17][CH:16]=2)=[O:13])[N:10]=[C:6]1[C:4]([OH:5])=[O:3]

참가 물질

6

반응물 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 59421902Ethyl 1-methyl-4-[({[4-(trifluoromethoxy)phenyl]amino}carbonyl)amino]-1H-imidazole-2-carboxylate

생성물 1

HCID 594218021-Methyl-4-[({[4-(trifluoromethoxy)phenyl]amino}carbonyl)amino]-1H-imidazole-2-carboxylic Acid

시약·촉매·용매 2

HCID 702Ethanol용매HCID 8028Tetrahydrofuran용매

실험 절차

835 mg (2.13 mmol) of 1-methyl-4-[({[4-(trifluoromethoxy)phenyl]-amino}carbonyl)amino]-1H-imidazole-2-carboxylic acid ethyl ester (Example 3A) is suspended in 5 ml of ethanol and 12 ml of tetrahydrofuran. While being cooled with ice, 2 ml (25 mmol) of 50% aqueous sodium hydroxide solution is added. The reaction mixture is stirred overnight at room temperature and then made acidic with 1N hydrochloric acid while being cooled with ice. The solution is extracted with dichloromethane. The organic phase is concentrated by evaporation in a vacuum. The residue is purified by preparative HPLC.

후처리

  1. additionis added
  2. temperaturewhile being cooled with ice
  3. extractionThe solution is extracted with dichloromethane
  4. concentrationThe organic phase is concentrated by evaporation in a vacuum
  5. customThe residue is purified by preparative HPLC

출처 및 근거

ORD 기록
ord-1661679caa5c46de99a31372b2624242
출처 데이터셋
uspto-grants-2015_09
특허 번호
US09133165B2

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