HRID1453803

反应详情

EQUATION

反应方程式

HRID 1453803 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
70 °C

PROCEDURE

实验过程

To a gently heated (35° C.) and mechanically stirred suspension of isonicotinohydrazide (435 g) in isopropyl alcohol (6.0 L) was added (methylimino)(thioxo)methane (230 g) in several small portions. After complete addition, the reaction mixture was heated (70° C.) for 6 h with an additional addition of isopropyl alcohol (600 ml) after 30 min. After cooling (ice-bath) the reaction mixture to 17° C., the obtained precipitate was filtered off and washed with isopropyl alcohol (1.0 L). This solid was then air-dried over night to provide 615 g of the title compound as a white powder.

WORKUP

后处理

  1. temperatureTo a gently heated
  2. additionAfter complete addition
  3. temperatureAfter cooling (ice-bath) the reaction mixture to 17° C.
  4. filtrationthe obtained precipitate was filtered off
  5. washwashed with isopropyl alcohol (1.0 L)
  6. customThis solid was then air-dried over night