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
PROCEDURE
实验过程
A mixture of 7-[(6-chloro[1,2,4]triazolo[4,3-b]pyridazin-3-yl)methoxy]furo[3,2-c]pyridin-6-amine (15.0 mg, 0.047 mmol), 1-methyl-4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)-1H-pyrazole (19.7 mg, 0.095 mmol), Pd(PPh3)4 (5 mg, 0.004 mmol), potassium carbonate (19.6 mg, 0.142 mmol) and 4:1 dioxane:water (2 mL) was microwaved at 100° C. for 30 min. The solution was loaded into a SCX cartridge, washed with MeOH and ejected with 2M NH3 in MeOH. The filtrate was concentrated in vacuo, redissolved in MeOH (0.5 mL) and purified via HPLC. The fractions containing the pure product were concentrated in vacuo to afford the title compound as a white solid. MS (ES+): m/z 363.06 (100) [MH+]. HPLC: tR=1.89 min (ZQ3, polar—5 min).
WORKUP
后处理
- washwashed with MeOH
- concentrationThe filtrate was concentrated in vacuo
- dissolutionredissolved in MeOH (0.5 mL)
- custompurified via HPLC
- additionThe fractions containing the pure product
- concentrationwere concentrated in vacuo