반응 #220671

반응 방정식

aminoguanidine bicarbonate

methanesulfonic acid

→

Aminoguanidine Dimesylate

용매

methanol

반응 조건

후처리

1. 1
   기타equipped with a magnetic stirrer
2. 2
   기타to rise to 40-45° C
3. 3
   workup.ADDITIONAfter the addition the obtained solution
4. 4
   온도cooled to (−3)-(−5) ° C
5. 5
   workup.STIRRINGand stirred at this temperature for 1 h
6. 6
   여과The precipitated crystals are filtered off
7. 7
   세척washed with 6.8 ml of methanol of (−3)-(−5) ° C

실험 절차

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.

출처