Ammonium Acetate → HCID 178489917, 화합물

HRID 2235686노트

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HRID 2235686 반응식
[F:1][C:2]1[CH:29]=[CH:28][C:5]([CH2:6][C:7]2O[C:9](/[CH:12]=[CH:13]/[C:14]3[CH:19]=[CH:18][C:17]([N:20]4[CH:24]=[C:23]([CH3:25])[N:22]=[CH:21]4)=[C:16]([O:26][CH3:27])[CH:15]=3)=[N:10][N:11]=2)=[CH:4][CH:3]=1.C([O-])(=O)C.[NH4+:34]>C(O)(=O)C>[F:1][C:2]1[CH:29]=[CH:28][C:5]([CH2:6][C:7]2[NH:34][C:9](/[CH:12]=[CH:13]/[C:14]3[CH:19]=[CH:18][C:17]([N:20]4[CH:24]=[C:23]([CH3:25])[N:22]=[CH:21]4)=[C:16]([O:26][CH3:27])[CH:15]=3)=[N:10][N:11]=2)=[CH:4][CH:3]=1

참가 물질

4

반응물 2

HCID 517165Ammonium AcetateHCID 670674112-(4-fluorobenzyl)-5-{(E)-2-[3-methoxy-4-(4-methyl-1H-imidazol-1-yl)phenyl]vinyl}-[1,3,4]oxadiazole

생성물 1

HCID 178489917HCID 178489917, 화합물수율 61.7%

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

A solution of 2-(4-fluorobenzyl)-5-{(E)-2-[3-methoxy-4-(4-methyl-1H-imidazol-1-yl)phenyl]vinyl}-[1,3,4]oxadiazole (65 mg) and ammonium acetate (256 mg) in acetic acid (1 mL) was stirred at 150° C. for four 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). The resulting solid was suspended in diethyl ether and collected by filtration to obtain 40 mg of the title compound. The property values of the compound are as follows.

후처리

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

출처 및 근거

ORD 기록
ord-576e2824fb4a493db696e954a4984a09
출처 데이터셋
uspto-grants-2010_05
특허 번호
US07713993B2

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