Hydrochloric Acid → (4E)-4-phenyl-4-[[4-[(5-phenylimidazo[1,2-a]pyridin-2-yl)methoxy]phenyl]methoxyimino]butanoic acid

HRID 1070131노트

반응식

HRID 1070131 반응식
[OH-].[Na+].[C:3]1([C:9]2[N:14]3[CH:15]=[C:16]([CH2:18][O:19][C:20]4[CH:41]=[CH:40][C:23]([CH2:24][O:25]/[N:26]=[C:27](/[C:34]5[CH:39]=[CH:38][CH:37]=[CH:36][CH:35]=5)\[CH2:28][CH2:29][C:30]([O:32]C)=[O:31])=[CH:22][CH:21]=4)[N:17]=[C:13]3[CH:12]=[CH:11][CH:10]=2)[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1.CO.Cl>O1CCCC1>[C:3]1([C:9]2[N:14]3[CH:15]=[C:16]([CH2:18][O:19][C:20]4[CH:21]=[CH:22][C:23]([CH2:24][O:25]/[N:26]=[C:27](/[C:34]5[CH:35]=[CH:36][CH:37]=[CH:38][CH:39]=5)\[CH2:28][CH2:29][C:30]([OH:32])=[O:31])=[CH:40][CH:41]=4)[N:17]=[C:13]3[CH:12]=[CH:11][CH:10]=2)[CH:4]=[CH:5][CH:6]=[CH:7][CH:8]=1

참가 물질

6

실험 절차

A 1N aqueous saturated solution of sodium hydroxide (5 ml) was added to a solution of methyl E-4-[4-(5-phenylimidazo[1,2-α]pyridin-2-ylmethoxy)benzyloxyimino]-4-phenylbutyrate (400 mg) in tetrahydrofuran (10 ml)-methanol (5 ml) and stirred at room temperature for 1 hour. 1N hydrochloric acid (5.5 ml) was added to the reaction mixture and extracted with ethyl acetate. The ethyl acetate layer was washed with an aqueous saturated solution of sodium chloride, dried (MgSO4) and concentrated. The residue was recrystallized from ethyl acetate-hexane to obtain E-4-[4-(5-phenylimidazo[1,2-α]pyridin-2-ylmethoxy)benzyloxyimino]-4-phenylbutyric acid (365 mg, yield 94%) as colorless crystals. m.p. 160-161° C.

후처리

  1. extractionextracted with ethyl acetate
  2. washThe ethyl acetate layer was washed with an aqueous saturated solution of sodium chloride
  3. dry with materialdried (MgSO4)
  4. concentrationconcentrated
  5. customThe residue was recrystallized from ethyl acetate-hexane

출처 및 근거

ORD 기록
ord-782db8e523a04a53a45c4f145d2bb486
출처 데이터셋
uspto-grants-2001_06
특허 번호
US06251926B1

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