Sodium Chloride → HCID 21200215, compound
Reaction equation
[OH-:1].[Na+].C([CH:5]([CH2:9][C:10](Cl)=[O:11])[C:6](Cl)=[O:7])C.[Cl-].[Na+].[N:15]1[CH:20]=[CH:19][C:18]([N:21]2[CH2:26][CH2:25][NH:24][CH2:23][CH2:22]2)=[CH:17][CH:16]=1>>[O:11]=[C:10]([N:24]1[CH2:23][CH2:22][N:21]([C:18]2[CH:19]=[CH:20][N:15]=[CH:16][CH:17]=2)[CH2:26][CH2:25]1)[CH2:9][CH2:5][C:6]([OH:7])=[O:1]Participants
Procedure
To an aqueous solution (10 ml) of 1-(4-pyridyl)-piperazine (1.63 g) were added 2N sodium hydroxide (5.5 ml) and ethylsuccinyl chloride at 0° C. and the solution was stirred for 1 hour at room temperature 1 hour. The reaction solution was saturated with sodium chloride, extracted with ethyl acetate three times and dried over Na2SO4. The solution was removed under reduced pressure and the residue was dissolved in methanol (10 ml). To the solution was added 2N sodium hydroxide (11 ml) and the solution was stirred for 1 hour at room temperature. The pH of the reaction mixture was adjusted to 5 with acetic acid and the solution was concentrated under reduced pressure and the concentrate was recrystallized from ethanol to give the titled compound (1.4 g) as a colorless crystal.
Workup
- extractionextracted with ethyl acetate three times
- dry with materialdried over Na2SO4
- customThe solution was removed under reduced pressure
- dissolutionthe residue was dissolved in methanol (10 ml)
- additionTo the solution was added 2N sodium hydroxide (11 ml)
- stirringthe solution was stirred for 1 hour at room temperature
- concentrationthe solution was concentrated under reduced pressure
- customthe concentrate was recrystallized from ethanol
Sources & evidence
- ORD record
- ord-dc7869dc14534778ad41f56ae10cf4e0
- Source dataset
- uspto-grants-2001_06
- Patent number
- US06242600B1
Reaction notes
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