Difluoroacetic acid → 6-Chloro-3-(difluoromethyl)-[1,2,4]triazolo[4,3-b]pyridazine

HRID 1674760

反応式

HRID 1674760 の反応式
[Cl:1][C:2]1[N:3]=[N:4][C:5]([NH:8][NH2:9])=[CH:6][CH:7]=1.[F:10][CH:11]([F:15])[C:12](O)=O>>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]2[N:4]([C:12]([CH:11]([F:15])[F:10])=[N:9][N:8]=2)[N:3]=1

参加物

3

反応物 2

HCID 9788Difluoroacetic acidHCID 1007873-Chloro-6-hydrazinopyridazine

生成物 1

HCID 14723856-Chloro-3-(difluoromethyl)-[1,2,4]triazolo[4,3-b]pyridazine収率 84.7%

反応条件

温度
100 °C

実験手順

A mixture of 3-chloropyridazin-6-yl hydrazine (5.0 g, 34.72 mmol) and difluoroacetic acid (21.93 mL; ca. 347 mmol) was heated at 100° C. for 3 hours and then evaporated to dryness. The involatile residue was dissolved in ethyl acetate (200 mL) and washed sequentially with saturated aqueous sodium carbonate and then saturated brine. The organic phase was dried over MgSO4, filtered, and evaporated to give 6-chloro-3-difluoromethyl-[1,2,4]-triazolo[4,3-b]pyridazine (6.0 g, 84.7%) as a white solid that was used without further purification.

後処理

  1. customevaporated to dryness
  2. dissolutionThe involatile residue was dissolved in ethyl acetate (200 mL)
  3. washwashed sequentially with saturated aqueous sodium carbonate
  4. dry with materialThe organic phase was dried over MgSO4
  5. filtrationfiltered
  6. customevaporated

出典と根拠

ORDレコード
ord-0ceaf4b1da1f4d33957a3227a815b9d9
出典データセット
uspto-grants-2011_08
特許番号
US08003649B2

関連ノート

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