1-Ethylpiperazine → 4-Ethylpiperazine-1-sulfonamide
Reaction equation
[CH2:1]([N:3]1[CH2:8][CH2:7][NH:6][CH2:5][CH2:4]1)[CH3:2].[S:9](N)([NH2:12])(=[O:11])=[O:10]>O1CCOCC1>[CH2:1]([N:3]1[CH2:8][CH2:7][N:6]([S:9]([NH2:12])(=[O:11])=[O:10])[CH2:5][CH2:4]1)[CH3:2]Participants
4
Reactant 2
Product 1
Reagents, catalysts & solvents 1
Procedure
A solution of N-ethylpiperazine (5.0 g) and sulfamide (10.0 g) in 1,4-dioxane (100 ml) was stirred for 72 h at 110° C. The volatiles were removed in vacuo and 5 g of the residue was dissolved in methanol and applied to an SCX cartridge (70 g). The cartridge was washed with 50% aqueous methanol (200 ml) before the subtitle product was eluted with 10% triethylamine/methanol (100 ml) The solvent was removed under reduced pressure to yield the subtitle compound as a pale beige solid. Yield: 3.0 g.
Workup
- customThe volatiles were removed in vacuo and 5 g of the residue
- dissolutionwas dissolved in methanol
- washThe cartridge was washed with 50% aqueous methanol (200 ml) before the subtitle product
- washwas eluted with 10% triethylamine/methanol (100 ml) The solvent
- customwas removed under reduced pressure
Sources & evidence
- ORD record
- ord-805bd304b43a4829b8e8a3645cca3048
- Source dataset
- uspto-grants-2012_01
- Patent number
- US08106063B2
Reaction notes
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