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Piperazine → HCID 20299635, compound

HRID 1733470
Notes
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Reaction equation

HRID 1733470 reaction equation
Cl[C:2]1[N:3]=[CH:4][C:5]2[N:6]([C:8]([S:11][C:12]([F:15])([F:14])[F:13])=[CH:9][N:10]=2)[CH:7]=1.[NH:16]1[CH2:21][CH2:20][NH:19][CH2:18][CH2:17]1>C(#N)C>[N:16]1([C:2]2[N:3]=[CH:4][C:5]3[N:6]([C:8]([S:11][C:12]([F:15])([F:14])[F:13])=[CH:9][N:10]=3)[CH:7]=2)[CH2:21][CH2:20][NH:19][CH2:18][CH2:17]1
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

4

Reactant 2

HCID 4837PiperazineHCID 20299638HCID 20299638, compound

Product 1

HCID 20299635HCID 20299635, compound

Reagents, catalysts & solvents 1

HCID 6342AcetonitrileSolvent

Procedure

6-Chloro-3-trifluoromethylthioimidazo[1,2-a]pyrazine from Step A is reacted with piperazine (2 g) in efluxing acetonitrile for 24 hours. The mixture is cooled, concentrated under vacuum, and the esidue partitioned between dilute sodium hydroxide and chloroform. The chloroform extract is dried over sodium sulfate, filtered and concentrated under vacuum to the crude base which is purified by chromatography on silica gel and converted to 6-(1-piperazinyl)-3-trifluoromethylthioimidazo[1,2-a]pyrazine hydrochloride with ethanolic hydrogen chloride.

Workup

  1. customfor 24 hours
  2. temperatureThe mixture is cooled
  3. concentrationconcentrated under vacuum
  4. customthe esidue partitioned between dilute sodium hydroxide and chloroform
  5. extractionThe chloroform extract
  6. dry with materialis dried over sodium sulfate
  7. filtrationfiltered
  8. concentrationconcentrated under vacuum to the crude base which
  9. customis purified by chromatography on silica gel

Sources & evidence

ORD record
ord-7524e5751b054103995019081c48b783
Source dataset
uspto-grants-1980_12
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US04242344

Reaction notes

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On this pageParticipantsProcedureWorkupSources & evidenceReaction notes