Ethanol → HCID 178433518、化合物

HRID 1154853ノート

反応式

HRID 1154853 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](O)[CH3:13]>C(C(CC)(CC)C([O-])([O-])[O-])C>[N:1]1[CH:6]=[CH:5][CH:4]=[CH:3][C:2]=1[N:7]1[C:12]([CH3:13])=[N:11][C:9]([OH:10])=[N:8]1

参加物

4

反応物 2

HCID 702EthanolHCID 13366065Hydrazinecarboxamide, 2-(2-pyridinyl)-

生成物 1

HCID 178433518HCID 178433518、化合物

試薬・触媒・溶媒 1

HCID 21875354Triethylorthoaceate溶媒

実験手順

A reaction mixture was prepared by suspending 457.6 g (3 m) of 2-pyridinyl-hydrazine carboxamide in 2600 ml of triethylorthoacetate and the mixture refluxed for about 9 hours. The ethanol by-product formed was continuously removed by distillation allowing the reaction temperature to stay at 125°-130° C. The 1-(2-pyridinyl)-5-methyl-1H-1,2,4-triazol-3-ol product was recovered by filtration in a yield of 116 g (66 percent of theoretical) and was washed with chloroform. The product melted at 194°-195° C. and upon analysis was found to have carbon hydrogen and nitrogen contents of 53.87, 4.55 and 31.95 percent, respectively, as compared with the theoretical contents of 54.53, 4.57 and 31.80 percent, respectively, calculated for the above named compound.

後処理

  1. customA reaction mixture was prepared
  2. temperaturethe mixture refluxed for about 9 hours
  3. customwas continuously removed by distillation
  4. customto stay at 125°-130° C
  5. filtrationThe 1-(2-pyridinyl)-5-methyl-1H-1,2,4-triazol-3-ol product was recovered by filtration in a yield of 116 g (66 percent of theoretical)
  6. washwas washed with chloroform

出典と根拠

ORDレコード
ord-58c432bc1c06424b9e7bc30ff6a001b5
出典データセット
uspto-grants-1981_11
特許番号
US04298602

反応ノート

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