Ethyl orthoformate → HCID 178518009、化合物

HRID 544741ノート

反応式

HRID 544741 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

実験手順

A mixture of 31.9 g (0.21 m) of 2-pyridinyl- hydrazinecarboxamide 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 coled to 15° C. and the solid 1-(2-pyridinyl)-1H-1,2,4- -triazol-3ol 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. customwas coled to 15° C.
  6. filtrationthe solid 1-(2-pyridinyl)-1H-1,2,4- -triazol-3ol product was recovered by filtration
  7. washThe product after washing with methylene chloride
  8. customwas recovered in a yield of 25.2 g (74 percent of theoretical)

出典と根拠

ORDレコード
ord-a2a063a0a77a40eb88e3e58978508740
出典データセット
uspto-grants-1984_05
特許番号
US04451653

反応ノート

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