Diethyl Ether → HCID 178505340, compound

HRID 2361853Notes

Reaction equation

HRID 2361853 reaction equation
[CH3:1][S:2]([OH:5])(=[O:4])=[O:3].C(=O)(O)O.[NH2:10][NH:11][C:12]([NH2:14])=[NH:13].CCOCC>CO>[S:2]([OH:5])(=[O:4])(=[O:3])[CH3:1].[S:2]([OH:5])(=[O:4])(=[O:3])[CH3:1].[NH2:10][NH:11][C:12]([NH2:14])=[NH:13]

Participants

5

Reactant 3

HCID 3283Diethyl EtherHCID 6395Methanesulfonic AcidHCID 178513185HCID 178513185, compound

Product 1

HCID 178505340HCID 178505340, compound

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

To a stirred solution of 99.5% methanesulphonic acid [Aldrich] (422 g; 4.40 mol) in methanol (720 cm3) at 40° was added portionwise over 30 minutes aminoguanidine bicarbonate [Aldrich] (272.0 g; 2.00 mol). When the addition was complete, the solution was stirred until the temperature had fallen to ˜40° and then treated slowly with cold ether (500 cm3). During the addition, colourless needles started to deposit. The resulting slurry was stood at 0° for 4 hrs, filtered and the product washed with cold ether and dried overnight in vacuo at 50°. Yield=528 g (99.25%), mpt=149-150°

Workup

  1. additionWhen the addition
  2. customhad fallen to ˜40°
  3. additionDuring the addition, colourless needles
  4. filtrationfiltered
  5. washthe product washed with cold ether
  6. customdried overnight in vacuo at 50°

Sources & evidence

ORD record
ord-42e14b13691d43f6b22ea625727a7136
Source dataset
uspto-grants-2014_04
Patent number
US08691818B2

Reaction notes

Loading…