Reaktion #473875

Reaktionsgleichung

3-(3-{2-[(E)-3,5-diamino-6-chloro-pyrazine-2-carbonylimino]-1,3,8-triaza-spiro[4.5]decane-8-carbonyl}-benzenesulfonylamino)-propionic acid tert-butyl ester

3-(3-{2-[(E)-3,5-Diamino-6-chloro-pyrazine-2-carbonylimino]-1,3,8-triaza-spiro[4.5]decane-8-carbonyl}-benzenesulfonylamino)-propionic acid tert-butyl ester

Iso-hexane

→

title compound

3-(3-{2-[(E)-3,5-Diamino-6-chloro-pyrazine-2-carbonylimino]-1,3,8-triaza-spiro[4.5]decane-8-carbonyl}-benzenesulfonylamino)-propionic acid

Lösungsmittel

HCl

dioxane

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigeresulting suspension
2. 2
   Sonstigewas sonicated for 1 hour at RT
3. 3
   SonstigeThe solvent was decanted off
4. 4
   Waschenthe solids washed with iso-hexane (10×25 ml)
5. 5
   SonstigeThe resulting pale yellow crystals were dried under vacuum @45° C. for 36 h

Vorschrift

A solution of 3-(3-{2-[(E)-3,5-diamino-6-chloro-pyrazine-2-carbonylimino]-1,3,8-triaza-spiro[4.5]decane-8-carbonyl}-benzenesulfonylamino)-propionic acid tert-butyl ester (step 1) (900 mg, 1.415 mmol) in 4N HCl in dioxane (10 ml) was stirred for 16 h at RT. Iso-hexane (10 ml) was added to the reaction mixture and resulting suspension was sonicated for 1 hour at RT. The solvent was decanted off and the solids washed with iso-hexane (10×25 ml). The resulting pale yellow crystals were dried under vacuum @45° C. for 36 h to afford the title compound; LC-MS Rt 0.80 mins; 580.0 [M+H]+, Method 2minLC_v003.

Quelle