HRID259550

反应详情

EQUATION

反应方程式

HRID 259550 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. additionAt 60°-65° C., there was added slowly a solution of 10.8 g
  2. customAfter 1 hour at 60°-65° C. the solvent was evaporated
  3. extractionthe residue was extracted with hot benzene and acetic acid
  4. customThe benzene was decanted
  5. temperaturecooled
  6. customto give a precipitate
  7. customRecrystallization from methanol