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

HRID 26648노트

반응식

HRID 26648 반응식
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

참가 물질

4

반응물 2

HCID 702762-Methylbenzoyl chlorideHCID 178486233HCID 178486233, 화합물

생성물 1

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

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

반응 조건

온도
120 °C

실험 절차

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%.

후처리

  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

출처 및 근거

ORD 기록
ord-7bda1585673340e6b793222737cca3f5
출처 데이터셋
uspto-grants-1979_04
특허 번호
US04151169

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