反应详情

N-(1-Aza-bicyclo[2.2.2]oct-3-yl)-N′-(3,5-diamino-6-chloro-pyrazine-2-carbonyl)-guanidine (Intermediate 4, 152 mg, content ca. 66%, 0.30 mmol) and 3,4,5-trimethoxybenzyl chloride (Aldrich, 77 mg, 0.36 mmol) is stirred in DMF (1 mL) at r.t. for ca. 18 h. The crude mixture is purified by preparative HPLC (5 mM ammonium formate in H2O: CH3CN gradient). The product thus obtained is triturated with a mixture of diethyl ether (4 mL) and methanol (1.5 mL), collected by filtration and dried under vacuum at 70° C. Further trituration with water (0.3 mL), filtration and drying under vacuum at 70° C. yields the title compound (35 mg).

1. customThe crude mixture is purified by preparative HPLC (5 mM ammonium formate in H2O: CH3CN gradient)
2. customThe product thus obtained
3. customis triturated with a mixture of diethyl ether (4 mL) and methanol (1.5 mL)
4. filtrationcollected by filtration
5. customdried under vacuum at 70° C
6. filtrationFurther trituration with water (0.3 mL), filtration
7. customdrying under vacuum at 70° C.