HRID30107
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
- 0 °C
PROCEDURE
实验过程
4-[6-Amino-5-(2-fluoro-benzoyl)-pyridin-2-ylamino]-piperidine-1-carboxylic acid tert-butyl ester (269.6 mg, 0.6504 mmol, Example 8) was dissolved in dichloromethane (5 mL), cooled to 0° C. and treated with trifluoroacetic acid (2.5 mL). After stirring ˜30 minutes, the reaction mixture was concentrated in vacuo. The salt was then neutralized with saturated sodium carbonate (˜3 mL), extracted with ethyl acetate/methylene chloride (˜50 mL), washed with saturated sodium chloride (˜3 mL), dried over sodium sulfate and evaporated in vacuo to give [2-Amino-6-(piperidin-4-ylamino)-pyridin-3-yl]-(2-fluoro-phenyl)-methanone as an off-white solid (200 mg, 0.636 mmol, 98 % yield).
WORKUP
后处理
- concentrationthe reaction mixture was concentrated in vacuo
- extractionextracted with ethyl acetate/methylene chloride (˜50 mL)
- washwashed with saturated sodium chloride (˜3 mL)
- dry with materialdried over sodium sulfate
- customevaporated in vacuo