反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 100 °C
PROCEDURE
实验过程
2-Chloro-5,6a-dimethyl-4-morpholino-6a,7,9,10-tetrahydro-[1,4]oxazino[3,4-h]pteridin-6(5H)-one (23 mg, 0.065 mmol), 1-methyl-3-(4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)phenyl)urea (21.54 mg, 0.078 mmol), PdCl2(dppf) (9.51 mg, 0.013 mmol) and sodium bicarbonate (1.5 mL, sat.) were mixed in 1,4-dioxane (3 mL). The suspension was heated by microwave irradiation at 100° C. for 30 minutes. After filtration, the solution was purified by mass-triggered preparative HPLC eluted with 20-25% of ACN (containing 0.035% TFA) in water (containing 0.05% TFA) on a Phenomenex Gemini 5 μm C18, 75×30 mm column) to give the title compound (5.3 mg 17% yield) as a pale yellow solid. 1H NMR (400 MHz, MeOD) δ ppm 1.57 (s, 3H) 2.70 (s, 3H) 2.80 (s, 3H) 3.34 (m, 1H) 3.64 (m, 1H) 3.72-3.86 (m, 9H) 4.10 (m, 2H) 4.25 (m, 1H) 7.51 (d, J=8 Hz, 2H) 7.62 (d, J=8 Hz, 2H). MS [M+H] Found 468.
WORKUP
后处理
- filtrationAfter filtration
- customthe solution was purified by mass-triggered preparative HPLC
- washeluted with 20-25% of ACN (containing 0.035% TFA) in water (containing 0.05% TFA) on a Phenomenex Gemini 5 μm C18, 75×30 mm column)