Reaktion #567848

Reaktionsgleichung

3-chloro-3-methyl-2-nitrosobutane

tris-(2-aminoethyl)amine

sodium bicarbonate

→

Compound 15

Ausbeute 9.5%

3,3,11,11-tetramethyl-7-aminoethyl-4,7,10-triazatridecane-2,12-dionedioxime

Ausbeute 9.5%

Lösungsmittel

acetonitrile

acetonitrile

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.WAITThe reaction mixture was left
2. 2
   Filtrationfiltered
3. 3
   WaschenThe residue was washed well with acetonitrile
4. 4
   Sonstigethe filtrate evaporated
5. 5
   SonstigeThe crude product was then purified by RP-HPLC (System L)

Vorschrift

To a solution of tris-(2-aminoethyl)amine (1 ml, 6.68 mmol) in acetonitrile (10 ml) was added sodium bicarbonate (1.12 g, 13.36 mmol, 2 eq). A solution of 3-chloro-3-methyl-2-nitrosobutane (1.359 g, 10.02 mmol, 1.5 eq) in dry acetonitrile (5 ml) was added slowly. The reaction mixture was left to stir at room temperature for 3 days, and then filtered. The residue was washed well with acetonitrile, and the filtrate evaporated. The crude product was then purified by RP-HPLC (System L) to afford Compound 15 (164 mg, 7%).

Quelle