Ethyl orthoformate → HCID 178518009、化合物

HRID 2198401ノート

反応式

HRID 2198401 の反応式
[N:1]1[CH:6]=[CH:5][CH:4]=[CH:3][C:2]=1[NH:7][NH:8][C:9]([NH2:11])=[O:10].[CH2:12](OC(OCC)OCC)C>C(O)C>[N:1]1[CH:6]=[CH:5][CH:4]=[CH:3][C:2]=1[N:7]1[CH:12]=[N:11][C:9]([OH:10])=[N:8]1

参加物

4

反応物 2

HCID 31214Ethyl orthoformateHCID 13366065Hydrazinecarboxamide, 2-(2-pyridinyl)-

生成物 1

HCID 178518009HCID 178518009、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
15 °C

実験手順

A mixture of 31.9 g (0.21 m) of 2-pyridinylhydrazinecarboxamide and 17.50 ml of triethylorthoformate was refluxed for 6 hours with the ethanol formed as a by-product being continuously removed by distillation thereby maintaining the reaction temperature at 130°-140° C. At the completion of the reaction, the reaction mixture was cooled to 15° C. and the solid 1-(2-pyridinyl)-1H-1,2,4-triazol-3-ol product was recovered by filtration. The product after washing with methylene chloride was recovered in a yield of 25.2 g (74 percent of theoretical). The product melted at 260°-262° C. and upon analysis was found to have carbon, hydrogen and nitrogen contents of 52.26, 3.90 and 34.79 percent, respectively, as compared with the theoretical contents of 51.89, 3.73 and 34.55 percent, respectively, calculated for the above named compound.

後処理

  1. customformed as a by-product being
  2. customcontinuously removed by distillation
  3. temperaturethereby maintaining the reaction temperature at 130°-140° C
  4. customAt the completion of the reaction
  5. filtrationthe solid 1-(2-pyridinyl)-1H-1,2,4-triazol-3-ol product was recovered by filtration
  6. washThe product after washing with methylene chloride
  7. customwas recovered in a yield of 25.2 g (74 percent of theoretical)

出典と根拠

ORDレコード
ord-30bfe8bab97e45389c4949b6e8748e9e
出典データセット
uspto-grants-1982_11
特許番号
US04357327

反応ノート

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