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

HRID 1351016ノート

反応式

HRID 1351016 の反応式
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]

参加物

4

反応物 3

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

生成物 1

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

実験手順

(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+).

後処理

  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

出典と根拠

ORDレコード
ord-f8903ad01ab040dba0f0a680aa170aa9
出典データセット
uspto-grants-2007_05
特許番号
USRE039634E1

反応ノート

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