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

HRID 1985632노트

반응식

HRID 1985632 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

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%.

후처리

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

출처 및 근거

ORD 기록
ord-7ee9207ad11b40b78e127985c5b2941d
출처 데이터셋
uspto-grants-2009_06
특허 번호
US07547698B2

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