Reacción #220671

ord-afa942980f3942349062cd5c6781afd5

Ecuación de reacción

N=C(N)NN.O=C(O)O
aminoguanidine bicarbonate
CS(=O)(=O)O
methanesulfonic acid
CS(=O)(=O)O.CS(=O)(=O)O.N=C(N)NN
Aminoguanidine Dimesylate

Disolventes

Condiciones de reacción

Temperatura
67.5°CELSIUS
Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

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

Procedimiento

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.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US07390899B2uspto-grants-2008_06