N'-acetyl-4-methyl-3-nitrobenzohydrazide → 2-Methyl-5-(4-methyl-3-nitrophenyl)-1,3,4-oxadiazole

HRID 1893544

반응식

HRID 1893544 반응식
[C:1]([NH:4][NH:5][C:6](=[O:17])[C:7]1[CH:12]=[CH:11][C:10]([CH3:13])=[C:9]([N+:14]([O-:16])=[O:15])[CH:8]=1)(=O)[CH3:2]>C(OCC)(=O)C>[CH3:2][C:1]1[O:17][C:6]([C:7]2[CH:12]=[CH:11][C:10]([CH3:13])=[C:9]([N+:14]([O-:16])=[O:15])[CH:8]=2)=[N:5][N:4]=1

참가 물질

3

반응물 1

HCID 47101699N'-acetyl-4-methyl-3-nitrobenzohydrazide

생성물 1

HCID 450976312-Methyl-5-(4-methyl-3-nitrophenyl)-1,3,4-oxadiazole수율 140.7%

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

반응 조건

온도
120 °C

실험 절차

The compound (0.70 g, 2.95 mmol) obtained in step A and polyphosphoric acid (8.0 g) were mixed, and the mixture was stirred with heating at 120° C. After cooling to room temperature, the reaction mixture was poured into ice water, and diluted with ethyl acetate. The mixture was washed with water and saturated aqueous sodium hydrogen carbonate, and dried over anhydrous magnesium sulfate. The insoluble material was filtered off, and the solution was concentrated under reduced pressure to give the title compound (0.91 g) as a colorless solid.

후처리

  1. temperatureAfter cooling to room temperature
  2. washThe mixture was washed with water and saturated aqueous sodium hydrogen carbonate
  3. dry with materialdried over anhydrous magnesium sulfate
  4. filtrationThe insoluble material was filtered off
  5. concentrationthe solution was concentrated under reduced pressure

출처 및 근거

ORD 기록
ord-aad2c1783bbc4c99a45d81fb94b6e2cc
출처 데이터셋
uspto-grants-2013_08
특허 번호
US08513235B2

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