Hydrochloric Acid → HCID 22344575, 화합물

HRID 1070128노트

반응식

HRID 1070128 반응식
[H-].[Na+].[OH:3]/[N:4]=[C:5](/[C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1)\[CH2:6][CH2:7][C:8]([O:10][CH3:11])=[O:9].[Cl:18][C:19]1[N:24]2[CH:25]=[C:26]([CH2:28][O:29][C:30]3[CH:35]=[CH:34][C:33]([CH2:36]Cl)=[CH:32][CH:31]=3)[N:27]=[C:23]2[CH:22]=[CH:21][CH:20]=1.Cl.C(=O)(O)[O-].[Na+]>CN(C)C=O.C(OCC)(=O)C.CCCCCC>[Cl:18][C:19]1[N:24]2[CH:25]=[C:26]([CH2:28][O:29][C:30]3[CH:31]=[CH:32][C:33]([CH2:36][O:3]/[N:4]=[C:5](/[C:12]4[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=4)\[CH2:6][CH2:7][C:8]([O:10][CH3:11])=[O:9])=[CH:34][CH:35]=3)[N:27]=[C:23]2[CH:22]=[CH:21][CH:20]=1

참가 물질

8

반응물 5

HCID 313Hydrochloric AcidHCID 24758Sodium hydrideHCID 516892Sodium BicarbonateHCID 12137371methyl (4E)-4-hydroxyimino-4-phenylbutanoateHCID 223445955-Chloro-2-(4-chloromethylphenoxymethyl)imidazo[1,2-a]pyridine

생성물 1

HCID 22344575HCID 22344575, 화합물수율 67%

시약·촉매·용매 2

HCID 6228Dimethylformamide용매HCID 21226206Ethyl acetate hexane용매

실험 절차

Sodium hydride (60%, in oil, 143 mg) was added to a solution of methyl E-4-(hydroxyimino)-4-phenylbutyrate (676 mg) and 5-chloro-2-(4-chloromethylphenoxymethyl)imidazo[1,2-α]pyridine (1.00 g) in N,N-dimethyformamide (10 ml) at room temperature and stirred for 1 hour. 1N hydrochloric acid (7 ml) was added, an aqueous saturated solution of sodium bicarbonate was added 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 subjected to silica gel chromatography to obtain methyl E-4-[4-(5-chloroimidazo[1,2-α]pyridin-2-ylmethoxy)benzyloxyimino]-4-phenylbutyrate (1.04 g, yield 67%) as a colorless oil from an ethyl acetate-hexane (2:1, v/v)-eluted fraction.

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

출처 및 근거

ORD 기록
ord-6b7c0d62ea0e4bf6ba4f6f445f8d471f
출처 데이터셋
uspto-grants-2001_06
특허 번호
US06251926B1

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