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

HRID 1351016노트

반응식

HRID 1351016 반응식
C(OC(=O)C(C)CCCCC[C:11]1([CH3:28])[N:15]=[C:14]([C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=2)[C:13]([C:22]2[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=2)=[N:12]1)C.[OH-:31].[Na+].[CH3:33][OH:34]>>[CH3:23][CH:22]([CH2:13][CH2:14][CH2:16][CH2:17][CH2:18][N:15]1[C:14]([C:16]2[CH:17]=[CH:18][CH:19]=[CH:20][CH:21]=2)=[C:13]([C:22]2[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=2)[N:12]=[C:11]1[CH3:28])[C:33]([OH:34])=[O:31]

참가 물질

4

반응물 3

HCID 887MethanolHCID 14798Sodium HydroxideHCID 694184432-Methyl-7-(2-methyl-4,5-diphenyl-imidazol-2-yl)-heptanoic acid ethyl ester

생성물 1

HCID 185375322-Methyl-7-(2-methyl-4,5-diphenyl-imidazol-1-yl)-heptanoic acid수율 99%

실험 절차

(Scheme 3 (P)) A solution of starting material 2-Methyl-7-(2-methyl-4,5-diphenyl-imidazol-2-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-f8903ad01ab040dba0f0a680aa170aa9
출처 데이터셋
uspto-grants-2007_05
특허 번호
USRE039634E1

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