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Piperazine → HCID 20299630, 화합물

HRID 1733472
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HRID 1733472 반응식
[Cl:1][C:2]1[N:3]=[CH:4][C:5]2[N:6]([C:8]([S:11](=[O:16])(=[O:15])[N:12]([CH3:14])[CH3:13])=[CH:9][N:10]=2)[CH:7]=1.[NH:17]1[CH2:22][CH2:21][NH:20][CH2:19][CH2:18]1>C(#N)C>[ClH:1].[CH3:13][N:12]([CH3:14])[S:11]([C:8]1[N:6]2[CH:7]=[C:2]([N:17]3[CH2:22][CH2:21][NH:20][CH2:19][CH2:18]3)[N:3]=[CH:4][C:5]2=[N:10][CH:9]=1)(=[O:16])=[O:15]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 4837PiperazineHCID 20299643HCID 20299643, 화합물

생성물 1

HCID 20299630HCID 20299630, 화합물

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

The crude product from Step A is reacted with piperazine (2 g) in refluxing acetonitrile for 18 hours and the mixture cooled and concentrated under vacuum, and the residue partitioned between dilute sodium hydroxide and chloroform. The chloroform extract is dried over sodium sulfate, filtered and concentrated under vacuum to a residue which is purified by chromatography on silica gel and crystallized from ethanolic hydrogen chloride to give 3-(N,N-dimethylsulfamoyl)-6-(1-piperazinyl)imidazo[1,2-a]pyrazine hydrochloride.

후처리

  1. temperaturethe mixture cooled
  2. concentrationconcentrated under vacuum
  3. customthe residue partitioned between dilute sodium hydroxide and chloroform
  4. extractionThe chloroform extract
  5. dry with materialis dried over sodium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated under vacuum to a residue which
  8. customis purified by chromatography on silica gel
  9. customcrystallized from ethanolic hydrogen chloride

출처 및 근거

ORD 기록
ord-ec569c351b934348847fc9da90dffafc
출처 데이터셋
uspto-grants-1980_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04242344

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