Sulfamide → (3R,5S)-3,5-dimethylpiperazine-1-sulfonamide
Reaktionsgleichung
[CH3:1][C@H:2]1[CH2:7][NH:6][CH2:5][C@@H:4]([CH3:8])[NH:3]1.[S:9](N)([NH2:12])(=[O:11])=[O:10]>O1CCOCC1>[CH3:8][C@H:4]1[NH:3][C@@H:2]([CH3:1])[CH2:7][N:6]([S:9]([NH2:12])(=[O:11])=[O:10])[CH2:5]1Komponenten
4
Edukt 2
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Versuchsvorschrift
A solution of cis-2,6-dimethylpiperazine (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 the residue suspended in EtOAc. The filtrate was evaporated to a yellow solid (4.3 g). 1 g of this material was dissolved in methanol and applied to an SCX cartridge (10 g). The cartridge was washed with 50% aqueous methanol (200 ml) before the subtitle product was eluted with 5% ammonium hydroxide solution/methanol (200 ml). The solvent was removed under reduced pressure to yield the subtitle compound as a yellow solid. Yield: 0.46 g.