Sodium Hydroxide → 2-Methyl-7-(2-methyl-4,5-diphenyl-imidazol-1-yl)-heptanoic acid

HRID 412206노트

반응식

HRID 412206 반응식
C([O:3][C:4](=[O:30])[CH:5]([CH3:29])[CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][N:11]1[C:15]([C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=2)=[C:14]([C:22]2[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=2)[N:13]=[C:12]1[CH3:28])C.[OH-].[Na+]>CO>[CH3:29][CH:5]([CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][N:11]1[C:15]([C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=2)=[C:14]([C:22]2[CH:23]=[CH:24][CH:25]=[CH:26][CH:27]=2)[N:13]=[C:12]1[CH3:28])[C:4]([OH:30])=[O:3]

참가 물질

4

반응물 2

HCID 14798Sodium HydroxideHCID 25190471ethyl 2-methyl-7-(2-methyl-4,5-diphenyl-1H-imidazol-1-yl)heptanoate

생성물 1

HCID 185375322-Methyl-7-(2-methyl-4,5-diphenyl-imidazol-1-yl)-heptanoic acid수율 99.6%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

(Scheme 3 (P)) A solution of starting material 2-Methyl-7-(2-methyl-4,5-diphenyl-imidazol-1-yl)-heptanoic acid ethyl ester (130 mg, 0.32 mmole) in Methanol (5 ml) and Sodium Hydroxide (64 mg, 1.61 mmole) was let stirred under reflux for 18 hrs. The next day, the reaction was let cooled to room temperature and concentrated in vacuo. The residue was diluted with water, and acidified with Hydrochloric Acid (3N). The aqueous layer was extracted with Dichloromethane (3×10 ml). The organic layers were combined, dried over Sodium Sulfate and filtered. The resultant filtrate was concentrated in vacuo to afford product as a white solid (120 mg, 99%). Mass Spec: 377 (MH+).

후처리

  1. temperatureunder reflux for 18 hrs
  2. concentrationconcentrated in vacuo
  3. additionThe residue was diluted with water
  4. extractionThe aqueous layer was extracted with Dichloromethane (3×10 ml)
  5. dry with materialdried over Sodium Sulfate
  6. filtrationfiltered
  7. concentrationThe resultant filtrate was concentrated in vacuo

출처 및 근거

ORD 기록
ord-cbfc84c7caf14d519d84168d860f03db
출처 데이터셋
uspto-grants-2003_05
특허 번호
US06562846B2

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