Methanesulfonic Acid → HCID 178505340, compound

HRID 133489Notes

Reaction equation

HRID 133489 reaction equation
C(=O)(O)O.[NH2:5][NH:6][C:7]([NH2:9])=[NH:8].[CH3:10][S:11]([OH:14])(=[O:13])=[O:12]>CO>[S:11]([OH:14])(=[O:13])(=[O:12])[CH3:10].[S:11]([OH:14])(=[O:13])(=[O:12])[CH3:10].[NH2:5][NH:6][C:7]([NH2:9])=[NH:8]

Participants

4

Reactant 2

HCID 6395Methanesulfonic AcidHCID 178513185HCID 178513185, compound

Product 1

HCID 178505340HCID 178505340, compound

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Conditions

Temperature
67.5 °C

Procedure

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

  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

Sources & evidence

ORD record
ord-afa942980f3942349062cd5c6781afd5
Source dataset
uspto-grants-2008_06
Patent number
US07390899B2

Reaction notes

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