HRID420669
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
- 80 °C
PROCEDURE
实验过程
A mixture of butyl 3-[2-[(2,2-dimethylpropanoyl)amino]-6-(methyloxy)-3-pyridinyl]propanoate (86.01 g, 256 mmol) in hydrochloric acid (500 ml, 3000 mmol) (6M aqueous), was heated at 80° C. for 6 h. Reaction was cooled, treated with water (500 ml), transferred to a 5 L conical flask and carefully neutralised with solid K2CO3 (requires around 250 g) (much effervescence was observed). The mixture was then extracted with 20% MeOH/DCM (3×500 ml). The combined organic solvents were then dried (MgSO4), filtered, evaporated to give the crude product as a yellow solid (35.84 g, 79%).
WORKUP
后处理
- customReaction
- temperaturewas cooled
- customtransferred to a 5 L conical flask
- extractionThe mixture was then extracted with 20% MeOH/DCM (3×500 ml)
- dry with materialThe combined organic solvents were then dried (MgSO4)
- filtrationfiltered
- customevaporated