HRID2065567
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
To a suspension of 5-[5-(4-methoxy-phenyl)-pyrimidin-2-ylamino]pyridine-2-carboxylic acid methyl ester 4 (0.3 mmol) in THF:MeOH:H2O=3:2:1 (5 mL), is added 6M LiOH (1.8 mmol). The reaction mixture is stirred at it for 12 h. After this time the solvent is removed under vacuum, the residue is diluted with H2O (6 mL) and the pH neutralized with 6M HCl. The solid that precipitates out is collected, washed with water and dried in a vacuum oven for 12 h to afford 5-[5-(4-methoxy-phenyl)-pyrimidin-2-ylamino]-pyridine-2-carboxylic acid 5 as a yellow solid, which is used in the next step without further purification. MS (m/z) (M+1)+: 323.2.
WORKUP
后处理
- customAfter this time the solvent is removed under vacuum
- additionthe residue is diluted with H2O (6 mL)
- customThe solid that precipitates out
- customis collected
- washwashed with water
- customdried in a vacuum oven for 12 h