Potassium Carbonate → HCID 178482546, compound
Reaction equation
[N:1]1([C:7]([O:9][C:10]([CH3:13])([CH3:12])[CH3:11])=[O:8])[CH2:6][CH2:5][NH:4][CH2:3][CH2:2]1.C(=O)([O-])[O-].[K+].[K+].Cl.Cl[CH2:22][C:23]1[N:24]([CH3:30])[C:25](=[N:28][CH3:29])[S:26][CH:27]=1>C(#N)C>[CH3:30][N:24]1[C:23]([CH2:22][N:4]2[CH2:5][CH2:6][N:1]([C:7]([O:9][C:10]([CH3:13])([CH3:12])[CH3:11])=[O:8])[CH2:2][CH2:3]2)=[CH:27][S:26]/[C:25]/1=[N:28]\[CH3:29]Participants
5
Procedure
tert-Butyl piperazine-1-carboxylate (2.5 g) was dissolved in acetonitrile (50 mL). Potassium carbonate (3.7 g) and N-(4-chloromethyl-3-methyl-1,3-thiazol-2(3H) -ylidene)-N-methylamine hydrochloride (3.2 g) were added thereto, and the mixture was mixed under reflux for 4 hours. The solvent was distilled off, and to the residue was added an aqueous potassium bicarbonate solution. The mixture was then extracted with chloroform, and the extract was dried over anhydrous magnesium sulfate. The solvent was distilled off, and the residue was purified with a basic silica gel column to give the title compound (4.3 g) as a brown oily matter.
Workup
- additionthe mixture was mixed
- temperatureunder reflux for 4 hours
- distillationThe solvent was distilled off
- additionto the residue was added an aqueous potassium bicarbonate solution
- extractionThe mixture was then extracted with chloroform
- dry with materialthe extract was dried over anhydrous magnesium sulfate
- distillationThe solvent was distilled off
- customthe residue was purified with a basic silica gel column
Sources & evidence
- ORD record
- ord-252ed28b501c45b3a8728622e1bb7e7d
- Source dataset
- uspto-grants-2009_05
- Patent number
- US07534887B2
Reaction notes
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