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
- 170 °C
PROCEDURE
实验过程
3-Amino-4-(2-hydroxy-2-methylpropylamino)quinoline (7.5 g, 32 mmol) was combined with methoxyacetic acid (7.5 mL, 97 mmol) and heated at about 170° C. for about 3 hours. The resulting solid residue was dissolved in ethyl acetate (150 mL). The ethyl acetate solution was extracted twice with 0.2N sodium hydroxide, washed with water, dried over magnesium sulfate, treated with activated charcoal and then concentrated to a volume of about 50 mL. Hexane was added to the ethyl acetate and the resulting precipitate was collected and dried to provide 0.9 g of the desired product as a crystalline solid, m.p. 145°-148° C. Analysis: Calculated: % C, 67.3; % H, 6.7; % N, 14.7; Found: % C, 67.2; % H, 6.6; % N, 14.6.
WORKUP
后处理
- extractionThe ethyl acetate solution was extracted twice with 0.2N sodium hydroxide
- washwashed with water
- dry with materialdried over magnesium sulfate
- additiontreated with activated charcoal
- concentrationconcentrated to a volume of about 50 mL
- additionHexane was added to the ethyl acetate
- customthe resulting precipitate was collected
- customdried