Ethyl Acetate → HCID 178489883, 화합물

HRID 599571노트

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HRID 599571 반응식
[F:1][C:2]1[CH:7]=[CH:6][C:5]([CH2:8][C:9](=O)[CH2:10][NH:11][C:12](=O)/[CH:13]=[CH:14]/[C:15]2[CH:20]=[CH:19][C:18]([N:21]3[CH:25]=[C:24]([CH3:26])[N:23]=[CH:22]3)=[C:17]([O:27][CH3:28])[CH:16]=2)=[CH:4][CH:3]=1.C([O-])(=O)C.[NH4+:35].C(OCC)(=O)C.O.C(=O)(O)[O-].[Na+]>C(O)(=O)C.C1(C)C(C)=CC=CC=1>[F:1][C:2]1[CH:7]=[CH:6][C:5]([CH2:8][C:9]2[N:35]=[C:12](/[CH:13]=[CH:14]/[C:15]3[CH:20]=[CH:19][C:18]([N:21]4[CH:25]=[C:24]([CH3:26])[N:23]=[CH:22]4)=[C:17]([O:27][CH3:28])[CH:16]=3)[NH:11][CH:10]=2)=[CH:4][CH:3]=1

참가 물질

7

반응물 4

HCID 8857Ethyl AcetateHCID 517165Ammonium AcetateHCID 67067457HCID 67067457, 화합물HCID 86585896Sodium bicarbonate water

생성물 1

HCID 178489883HCID 178489883, 화합물수율 31.7%

시약·촉매·용매 2

HCID 176Acetic Acid용매HCID 7237O-Xylene용매

실험 절차

A solution of (E)-N-[3-(4-fluorophenyl)-2-oxopropyl]-3-[3-methoxy-4-(4-methyl-1H-imidazol-1-yl)phenyl]acrylamide (43 mg) and ammonium acetate (163 mg) in acetic acid (1 mL) and xylene (5 mL) was heated under reflux for 16 hours. The reaction solution was left to cool to room temperature. Ethyl acetate and saturated sodium bicarbonate water were added to the reaction solution, and the organic layer was separated. The resulting organic layer was dried over anhydrous magnesium sulfate and then concentrated under reduced pressure. The residue was purified by silica gel column chromatography (carrier: Chromatorex™ NH; elution solvent: ethyl acetate→ethyl acetate:methanol=5:1) to obtain 13 mg of the title compound. The property values of the compound are as follows.

후처리

  1. temperatureunder reflux for 16 hours
  2. waitThe reaction solution was left
  3. customthe organic layer was separated
  4. dry with materialThe resulting organic layer was dried over anhydrous magnesium sulfate
  5. concentrationconcentrated under reduced pressure
  6. customThe residue was purified by silica gel column chromatography (carrier: Chromatorex™ NH; elution solvent: ethyl acetate→ethyl acetate:methanol=5:1)

출처 및 근거

ORD 기록
ord-9882cb93c2434ff893dda354da80195f
출처 데이터셋
uspto-grants-2011_03
특허 번호
US07897632B2

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