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 solution of 375 mg (1.09 mmol) 2-methyl-4-(3-methyl-1H-indazol-5-yl)-6-(trifluoromethyl)-1,4-dihydropyridine-3,5-dicarbonitrile (Example 4) in DMF (11.5 ml) was cooled to 0° C. 534 mg (1.64 mmol) caesium carbonate were added at this temperature, and after 15 min 48 μl (0.77 mmol) methyl iodide were added dropwise at room temperature. After stirring overnight at rt, additional methyl iodide (20 μl) and a small amount of caesium carbonate were added, and the reaction mixture was stirred at rt for further 3 h before water and methanol were added. The resulting solution was directly purified by preparative RP-HPLC (acetonitrile/water+0.1% TFA gradient) to give 75 mg (19% of th.) of the racemic title compound.
WORKUP
后处理
- additionwere added
- customThe resulting solution was directly purified by preparative RP-HPLC (acetonitrile/water+0.1% TFA gradient)