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
Diethylamine (0.400 mL) was suspended in tetrahydrofuran (2.00 mL) and cooled in an ice bath. This solution was charged with trimethylaluminum (0.500 mL of a 2 M solution in heptane). After 20 minutes the reaction was charged with the 2-(3-ethyl-ureido)-7-pyridin-3-yl-[1,2,4]triazolo[1,5-a]pyridine-5-carboxylic acid ethyl ester, prepared as in Example 16, Step 1, (0.255 g, 0.720 mmol) and shaken. After 18 hours the reaction was diluted with 1 volume of ethyl acetate and treated with an equal amount saturated aqueous sodium/potassium tartrate. After 6 hours the organic layer was isolated, dried over magnesium sulfate and concentrated to afford the desired product 2-(3-ethyl-ureido)-7-pyridin-3-yl-[1,2,4]triazolo[1,5-a]pyridine-5-carboxylic acid diethylamide, MS (APCI+): m/z 382.1 (M+H).
WORKUP
后处理
- temperaturecooled in an ice bath
- customAfter 6 hours the organic layer was isolated
- dry with materialdried over magnesium sulfate
- concentrationconcentrated