反应详情

A mixture of 35 mg (0.066 mmol) (S)-3-{3-[N′-(3,5-Diamino-6-chloro-pyrazine-2-carbonyl)-guanidino]-piperidin-1-ylmethyl}-benzoic acid methyl ester (intermediate 10) and 100 μl (0.7 mmol) methyl iodide in 2 ml acetone/dimethylformamide (1:1) is stirred at room temperature overnight. Then the reaction mixture is concentrated under reduced pressure and the residue is purified by preparative reverse phase HPLC (gradient of methanol and water+0.2% trifluoroacetic acid, 25° C.). Fractions containing the title compound were concentrated under reduced pressure, treated with excess HCl in methanol and evaporated again.

1. concentrationThen the reaction mixture is concentrated under reduced pressure
2. customthe residue is purified by preparative reverse phase HPLC (gradient of methanol and water+0.2% trifluoroacetic acid, 25° C.)
3. additionFractions containing the title compound
4. concentrationwere concentrated under reduced pressure
5. additiontreated with excess HCl in methanol
6. customevaporated again