Hydrazinecarboxaldehyde → 6-(2-Thienyl)-1,2,4-triazolo[4,3-b]pyridazine

HRID 443514ノート

反応式

HRID 443514 の反応式
Cl[C:2]1[N:3]=[N:4][C:5]([C:8]2[S:9][CH:10]=[CH:11][CH:12]=2)=[CH:6][CH:7]=1.[CH:13]([NH:15][NH2:16])=O>C(O)CCC>[S:9]1[CH:10]=[CH:11][CH:12]=[C:8]1[C:5]1[CH:6]=[CH:7][C:2]2[N:3]([CH:13]=[N:15][N:16]=2)[N:4]=1

参加物

4

反応物 2

HCID 12229HydrazinecarboxaldehydeHCID 64047013-Chloro-6-(thiophen-2-yl)pyridazine

生成物 1

HCID 142879766-(2-Thienyl)-1,2,4-triazolo[4,3-b]pyridazine

試薬・触媒・溶媒 1

HCID 2631-Butanol溶媒

実験手順

A mixture of 1.0 g. of 3-chloro-6-(2-thienyl)pyridazine and 0.6 g. of formic acid hydrazide in 50 ml. of n-butyl alcohol is heated at the reflux temperature for 18 hours. The volatiles are removed and the residue is partitioned between dilute aqueous sodium hydroxide and methylene chloride. The organic layer is dried over anhydrous sodium sulfate, filtered and evaporated. The residue is recrystallized from methylene chloride:hexane to afford a tan solid. The solid is recrystallized from acetone:hexane to give 0.5 g. of the desired product as cream colored crystals, m.p. 155°-159° C.

後処理

  1. additionA mixture of 1.0 g
  2. customThe volatiles are removed
  3. customthe residue is partitioned between dilute aqueous sodium hydroxide and methylene chloride
  4. dry with materialThe organic layer is dried over anhydrous sodium sulfate
  5. filtrationfiltered
  6. customevaporated
  7. customThe residue is recrystallized from methylene chloride
  8. customhexane to afford a tan solid
  9. customThe solid is recrystallized from acetone
  10. customhexane to give 0.5 g

出典と根拠

ORDレコード
ord-42c1714a4b82460d998ac35c57546625
出典データセット
uspto-grants-1981_04
特許番号
US04260756

反応ノート

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