Piperazine → 6-Piperazin-1-ylimidazo[1,2-b]pyridazine-2-carboxylic acid ethyl ester

HRID 1985632ノート

反応式

HRID 1985632 の反応式
[CH2:1]([O:3][C:4]([C:6]1[N:7]=[C:8]2[CH:13]=[CH:12][C:11](Cl)=[N:10][N:9]2[CH:15]=1)=[O:5])[CH3:2].[NH:16]1[CH2:21][CH2:20][NH:19][CH2:18][CH2:17]1.C(=O)([O-])[O-].[K+].[K+]>C1(C)C=CC=CC=1>[CH2:1]([O:3][C:4]([C:6]1[N:7]=[C:8]2[CH:13]=[CH:12][C:11]([N:16]3[CH2:21][CH2:20][NH:19][CH2:18][CH2:17]3)=[N:10][N:9]2[CH:15]=1)=[O:5])[CH3:2]

参加物

5

反応物 3

HCID 4837PiperazineHCID 11430Potassium CarbonateHCID 2779714ethyl 6-chloroimidazo[1,2-b]pyridazine-2-carboxylate

生成物 1

HCID 668640036-Piperazin-1-ylimidazo[1,2-b]pyridazine-2-carboxylic acid ethyl ester

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

A mixture of 6-chloroimidazo[1,2-b]pyridazine-2-carboxylic acid ethyl ester (1.000 g, 4.432 mmol), piperizine (0.458 g, 5.318 mmol) and potassium carbonate (0.620 g, 4.485 mmol) in 50 mL of toluene was refluxed for 48 hours. The reaction mixture was concentrated in vacuo, diluted with water and extracted with ethyl acetate. The crude product, 6-piperazin-1-ylimidazo[1,2-b]pyridazine-2-carboxylic acid ethyl ester, obtained upon removal of solvent was used for next step reaction without further purification. Yield 1.016 g, 83%.

後処理

  1. temperaturewas refluxed for 48 hours
  2. concentrationThe reaction mixture was concentrated in vacuo
  3. additiondiluted with water
  4. extractionextracted with ethyl acetate

出典と根拠

ORDレコード
ord-7ee9207ad11b40b78e127985c5b2941d
出典データセット
uspto-grants-2009_06
特許番号
US07547698B2

反応ノート

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