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
- 50 °C
PROCEDURE
实验过程
An aqueous solution of sodium hydroxide (2 N, 3.0 mL, 1.5 mmol) was added to a solution of 4-amino-3-[2-methyl-5-(3-methyl-[1,2,4]oxadiazol-5-yl)-phenoxymethyl]-thieno[3,2-c]pyridine-7-carboxylic acid ethyl ester (0.33 g, 0.78 mmol) (from Example 54 supra) in tetrahydrofuran/methanol (3:1, 8 mL) and the mixture was heated at 50° C. for 1 day. The reaction mixture was concentrated and azeotroped with toluene. The solid residue was triturated with ethyl acetate. The solid was then suspended in water and treated with hydrochloric acid (1N). After stirring 30 minutes, the solid was collected, washed with water and dried to 4-amino-3-[2-methyl-5-(3-methyl-[1,2,4]oxadiazol-5-yl)-phenoxymethyl]-thieno[3,2-c]pyridine-7-carboxylic acid. (Yield 0.29 g, 94%).
WORKUP
后处理
- concentrationThe reaction mixture was concentrated
- customazeotroped with toluene
- customThe solid residue was triturated with ethyl acetate
- additiontreated with hydrochloric acid (1N)
- customthe solid was collected
- washwashed with water
- dry with materialdried to 4-amino-3-[2-methyl-5-(3-methyl-[1,2,4]oxadiazol-5-yl)-phenoxymethyl]-thieno[3,2-c]pyridine-7-carboxylic acid