反应详情

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.

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