Ammonium Acetate → HCID 178489915, 화합물

HRID 1009345노트

반응식

HRID 1009345 반응식
[F:1][C:2]1[CH:3]=[C:4]([C:8]2O[C:10](/[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)=[N:11][N:12]=2)[CH:5]=[CH:6][CH:7]=1.C([O-])(=O)C.[NH4+:33]>C(O)(=O)C>[F:1][C:2]1[CH:3]=[C:4]([C:8]2[NH:33][C:10](/[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)=[N:11][N:12]=2)[CH:5]=[CH:6][CH:7]=1

참가 물질

4

반응물 2

HCID 517165Ammonium AcetateHCID 670672252-(3-fluorophenyl)-5-{(E)-2-[3-methoxy-4-(4-methyl-1H-imidazol-1-yl)phenyl]vinyl}-[1,3,4]oxadiazole

생성물 1

HCID 178489915HCID 178489915, 화합물수율 58.2%

시약·촉매·용매 1

HCID 176Acetic Acid용매

반응 조건

온도
150 °C

실험 절차

A solution of 2-(3-fluorophenyl)-5-{(E)-2-[3-methoxy-4-(4-methyl-1H-imidazol-1-yl)phenyl]vinyl}-[1,3,4]oxadiazole (50 mg) and ammonium acetate (205 mg) in acetic acid (3 mL) was heated under reflux at 150° C. for 1.5 hours. The reaction solution was left to cool to room temperature and concentrated under reduced pressure. Ethyl acetate and saturated sodium bicarbonate water were added to the residue, 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 (elution solvent: ethyl acetate->ethyl acetate:methanol=5:1) to obtain 29 mg of the title compound. The property value of the compound is as follows.

후처리

  1. waitThe reaction solution was left
  2. temperatureto cool to room temperature
  3. concentrationconcentrated under reduced pressure
  4. additionEthyl acetate and saturated sodium bicarbonate water were added to the residue
  5. customthe organic layer was separated
  6. dry with materialThe resulting organic layer was dried over anhydrous magnesium sulfate
  7. concentrationconcentrated under reduced pressure
  8. customThe residue was purified by silica gel column chromatography (elution solvent: ethyl acetate->ethyl acetate:methanol=5:1)

출처 및 근거

ORD 기록
ord-141c811dc5d04047884ec97da82dd921
출처 데이터셋
uspto-grants-2011_07
특허 번호
US07973033B2

반응 노트

불러오는 중…