HRID133489

反应详情

EQUATION

反应方程式

HRID 133489 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
67.5 °C

PROCEDURE

实验过程

13.61 g (0.1 mol) of aminoguanidine bicarbonate is suspended in 36 ml of methanol at 20-22° C. in a 250 ml round bottom flask, equipped with a magnetic stirrer, a thermometer, a reflux condenser and a dropping funnel. 21.14 g (0.22 mol) of methanesulfonic acid is added dropwise to the suspension over a period of 1.5 h, while the temperature of the reaction is allowed to rise to 40-45° C. After the addition the obtained solution is stirred at 65-70° C. for 15 min, then cooled to (−3)-(−5) ° C. and stirred at this temperature for 1 h. The precipitated crystals are filtered off and washed with 6.8 ml of methanol of (−3)-(−5) ° C.

WORKUP

后处理

  1. customequipped with a magnetic stirrer
  2. customto rise to 40-45° C
  3. additionAfter the addition the obtained solution
  4. temperaturecooled to (−3)-(−5) ° C
  5. stirringand stirred at this temperature for 1 h
  6. filtrationThe precipitated crystals are filtered off
  7. washwashed with 6.8 ml of methanol of (−3)-(−5) ° C