反应详情

To a solution of 5-[3-({1-[2-(2-chloroethoxy)phenyl]cyclopropyl}amino)-2-oxopyrazin-1(2H)-yl]-N-cyclopropyl-2-fluoro-4-methylbenzamide (Example 318h, 100 mg) and methylamine, 40% by wt solution in water (0.1 mL) in dioxane (1 mL) was added potassium iodide (33.4 mg). The reaction mixture was stirred at room temperature overnight, then heated at 40° C. overnight. The reaction was heated at 50° C. for 48 h. Purification by preparative HPLC (Phenomenex Gemini, eluting with a gradient of acetonitrile in 0.2% (v/v) aqueous ammonia, followed by Xbridge column eluting with a gradient of acetonitrile in 0.2% (v/v) aqueous ammonia) gave the title compound as a solid (17 mg).

1. temperatureheated at 40° C. overnight
2. temperatureThe reaction was heated at 50° C. for 48 h
3. customPurification by preparative HPLC (Phenomenex Gemini
4. washeluting with a gradient of acetonitrile in 0.2% (v/v) aqueous ammonia
5. washeluting with a gradient of acetonitrile in 0.2% (v/v) aqueous ammonia)