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

HRID 443515
ノート
印刷プレビュー

反応式

HRID 443515 の反応式
Cl[C:2]1[N:3]=[N:4][C:5]([C:8]2[CH:12]=[CH:11][S:10][CH:9]=2)=[CH:6][CH:7]=1.[CH:13]([NH:15][NH2:16])=O>C(O)CCC>[S:10]1[CH:11]=[CH:12][C:8]([C:5]2[CH:6]=[CH:7][C:2]3[N:3]([CH:13]=[N:15][N:16]=3)[N:4]=2)=[CH:9]1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 12229HydrazinecarboxaldehydeHCID 135734813-Chloro-6-(3-thienyl)pyridazine

生成物 1

HCID 234675826-(3-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 1.5 g. of 3-chloro-6-(3-thienyl)pyridazine and 0.96 g. of formic acid hydrazide in 50 ml. of n-butyl alcohol is heated at the reflux temperature for 48 hours. The reaction mixture is concentrated free of volatiles and the residue is partitioned between dilute 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 give a solid. The solid is recrystallized from acetone-hexane to provide 1.0 g. of the product of the Example as a orange-cream solid, m.p. 189°-192° C.

このページの内容参加物実験手順後処理出典と根拠反応ノート

後処理

  1. additionA mixture of 1.5 g
  2. concentrationThe reaction mixture is concentrated free of volatiles
  3. customthe residue is partitioned between dilute 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-hexane
  8. customto give a solid
  9. customThe solid is recrystallized from acetone-hexane
  10. customto provide 1.0 g

出典と根拠

ORDレコード
ord-0b244675225c4bf0a2dab362cb9a6fc7
出典データセット
uspto-grants-1981_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04260756

反応ノート

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