2-Methylbenzoyl chloride → 1-Methyl-5-(o-tolyl)-3-phenyl-1,2,4-triazole

HRID 26648ノート

反応式

HRID 26648 の反応式
Cl.[CH3:2][NH:3][NH:4][C:5](=[NH:12])[C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1.[C:13]1([CH3:22])[C:14]([C:19](Cl)=O)=[CH:15][CH:16]=[CH:17][CH:18]=1>C(OCC)C>[CH3:2][N:3]1[C:19]([C:14]2[CH:15]=[CH:16][CH:17]=[CH:18][C:13]=2[CH3:22])=[N:12][C:5]([C:6]2[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=2)=[N:4]1

参加物

4

反応物 2

HCID 702762-Methylbenzoyl chlorideHCID 178486233HCID 178486233、化合物

生成物 1

HCID 218245451-Methyl-5-(o-tolyl)-3-phenyl-1,2,4-triazole収率 76%

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

反応条件

温度
120 °C

実験手順

A mixture of 0.56 g. of benzimidic acid 2-methylhydrazide hydrochloride and 3.8 g. of o-toluic acid chloride is heated under stirring at about 120° C. After cooling and addition of diethyl ether, the hydrochloride of the triazole is collected on filter and then suspended in a sodium bicarbonate aqueous solution. The free base is extracted with diethyl ether and the organic phase, after drying over sodium sulfate, is evaporated. The crude compound is purified by distillation at 160° C./0.1 mm Hg. Yield 76%.

後処理

  1. additionA mixture of 0.56 g
  2. temperatureAfter cooling
  3. customthe hydrochloride of the triazole is collected
  4. filtrationon filter
  5. extractionThe free base is extracted with diethyl ether
  6. dry with materialthe organic phase, after drying over sodium sulfate
  7. customis evaporated
  8. distillationThe crude compound is purified by distillation at 160° C./0.1 mm Hg

出典と根拠

ORDレコード
ord-7bda1585673340e6b793222737cca3f5
出典データセット
uspto-grants-1979_04
特許番号
US04151169

反応ノート

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