HRID66361
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
A solution of 5.5 g. of 3,5-dinitro-2-pyridone in 200 ml. of methanol was adjusted to pH 8 with ammonium hydroxide. At 60-65° C., there was added slowly a solution of 10.8 g. of sodium sulfide nonahydrate in 30 ml. of water. After 1 hour at 60-65° C. the solvent was evaporated and the residue was extracted with hot benzene and acetic acid to neutralize any sodium salt. The benzene was decanted and cooled to give a precipitate. Recrystallization from methanol gave 3-amino-5-nitro-2-pyridone, m.p. 200°-201° C.
WORKUP
后处理
- additionAt 60-65° C., there was added slowly a solution of 10.8 g
- customAfter 1 hour at 60-65° C. the solvent was evaporated
- extractionthe residue was extracted with hot benzene and acetic acid
- customThe benzene was decanted
- temperaturecooled
- customto give a precipitate
- customRecrystallization from methanol