Acetic Acid → HCID 53823840, 화합물

HRID 584457노트

반응식

HRID 584457 반응식
[CH3:1][C:2]1[O:6][C:5]([C:7]2[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=2)=[N:4][C:3]=1[CH2:13][O:14][C:15]1[CH:23]=[CH:22][C:18]([CH2:19][O:20][NH2:21])=[CH:17][CH:16]=1.O=[C:25]([C:33]1[CH:34]=[N:35][CH:36]=[CH:37][CH:38]=1)[CH2:26][CH2:27][C:28]([O:30][CH2:31][CH3:32])=[O:29].C(O)(=O)C.C([O-])(=O)C.[Na+]>C(OCC)(=O)C.CCCCCC.O.C(O)C>[CH3:1][C:2]1[O:6][C:5]([C:7]2[CH:8]=[CH:9][CH:10]=[CH:11][CH:12]=2)=[N:4][C:3]=1[CH2:13][O:14][C:15]1[CH:16]=[CH:17][C:18]([CH2:19][O:20][N:21]=[C:25]([C:33]2[CH:34]=[N:35][CH:36]=[CH:37][CH:38]=2)[CH2:26][CH2:27][C:28]([O:30][CH2:31][CH3:32])=[O:29])=[CH:22][CH:23]=1

참가 물질

8

반응물 4

HCID 176Acetic AcidHCID 517045Sodium AcetateHCID 4248889Ethyl 4-oxo-4-(pyridin-3-yl)butanoateHCID 223445934-(5-Methyl-2-phenyl4-oxazolylmethoxy)benzyloxyamine

생성물 1

HCID 53823840HCID 53823840, 화합물수율 73.3%

시약·촉매·용매 3

HCID 702Ethanol용매HCID 962Water용매HCID 21226206Ethyl acetate hexane용매

실험 절차

After a mixture of 4-(5-methyl-2-phenyl-4-oxazolylmethoxy)benzyloxyamine (500 mg), ethyl 4-oxo-4-(3-pyridyl)butyrate (367 mg), acetic acid (0.276 ml), sodium acetate (264 mg) and ethanol (20 ml) was heated to reflux for 20 hours, the mixture was cooled to room temperature. Water 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 subjected to silica gel chromatography to obtain ethyl 4-[4-(5-methyl-2-phenyl-4-oxazolylmethoxy)benzyloxyimino]-4-(3-pyridyl)butyrate (590 mg, yield 73%) as a colorless oil from an ethyl acetate-hexane (3:2, v/v)-eluted fraction.

후처리

  1. temperaturewas heated
  2. temperatureto reflux for 20 hours
  3. extractionextracted with ethyl acetate
  4. washThe ethyl acetate layer was washed with an aqueous saturated solution of sodium chloride
  5. dry with materialdried (MgSO4)
  6. concentrationconcentrated

출처 및 근거

ORD 기록
ord-688a59f27e7f4219acdd1f15fde1acde
출처 데이터셋
uspto-grants-2005_08
특허 번호
US06924300B2

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