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

HRID 1893544

反応式

HRID 1893544 の反応式
[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

参加物

3

反応物 1

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

反応条件

温度
120 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-aad2c1783bbc4c99a45d81fb94b6e2cc
出典データセット
uspto-grants-2013_08
特許番号
US08513235B2

関連ノート

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