HRID2397570
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
26 g. of 4-amino-6-chloro-2-methyl-5-nitropyridine-3-carboxylic acid ethyl ester (0.1 mol.) in 300 ml. of alcohol and 15 g. of triethylamine are treated with 7.3 g. of butylamine for 30 minutes at reflux temperature. After this time, the solution is evaporated to dryness and 100 ml. of ethyl acetate are added to the residue. The triethylammonium chloride is filtered off, the solvent is evaporated and the remaining oil recrystallized from methanol. The yield of 4-amino-6-butylamino-2-methyl-5-nitropyridine-3-carboxylic acid ethyl ester is 25 g. (84%), m.p. 74°-76° (methanol).
WORKUP
后处理
- customAfter this time, the solution is evaporated to dryness and 100 ml
- additionof ethyl acetate are added to the residue
- filtrationThe triethylammonium chloride is filtered off
- customthe solvent is evaporated
- customthe remaining oil recrystallized from methanol