HRID1802490
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
- 85 °C
PROCEDURE
实验过程
To a solution of N-[2,6-dichloro-4-(2-methyl-1,3-dioxolan-2-yl)phenyl]-10-ethoxypyrido[4,3-c]-1,6-naphthyridin-6-amine and N-[2,6-dichloro-4-(2-methyl-1,3-dioxolan-2-yl)phenyl]-10-methoxypyrido[4,3-c]-1,6-naphthyridin-6-amine (3.0 g) in THF (30 mL) was added 6 N HCl (20 mL) and the mixture was heated to 85° C. for 3.5 hr. After cooling to room temperature, the mixture was neutralized with saturated NaHCO3 and extracted with 1:1 THF/EtOAc. The precipitate between the organic and aqueous layers were collected and determined to be pure by LCMS. The organic layer was concentrated and purified by column chromatography (100% CH2Cl2 to 30% MeOH).
WORKUP
后处理
- temperatureAfter cooling to room temperature
- extractionextracted with 1:1 THF/EtOAc
- customThe precipitate between the organic and aqueous layers were collected
- concentrationThe organic layer was concentrated
- custompurified by column chromatography (100% CH2Cl2 to 30% MeOH)