Ethanol → HCID 178429414, compound

HRID 1070369Notes

Reaction equation

HRID 1070369 reaction equation
C(O)C.C(=O)(O)O.[NH2:8][C:9]([NH2:11])=[NH:10].[C:12](OCC)(=[O:17])[CH2:13][C:14]([CH3:16])=O>CCCCCC>[CH3:16][C:14]1[NH:8][C:9]([NH2:11])=[N:10][C:12](=[O:17])[CH:13]=1

Participants

5

Reactant 3

HCID 702EthanolHCID 8868Ethyl AcetoacetateHCID 286947Carbonic acid-guanidine (1:1)

Product 1

HCID 178429414HCID 178429414, compoundYield 186.9%

Reagents, catalysts & solvents 1

HCID 8058HexaneSolvent

Procedure

Into a 1 liter flask 600 ml of dried Ethanol and 91.89 g (0.51 mol) of Guanidine Carbonate and 146.1 g (1.11 mol) of ethyl acetoacetate were added. The reaction solution was gradually heated to reflux temperature and stirred overnight. 300 ml of Ethanol was evaporated and reaction solution was heated under reflux for two hours. After cooling, 300 ml of Hexane was added. Deposit was filtered, washed and dried. 119.3 g of 6-methylisocytosine was obtained.

Workup

  1. temperatureThe reaction solution was gradually heated
  2. temperatureto reflux temperature
  3. custom300 ml of Ethanol was evaporated
  4. customreaction solution
  5. temperaturewas heated
  6. temperatureunder reflux for two hours
  7. temperatureAfter cooling
  8. filtrationDeposit was filtered
  9. washwashed
  10. customdried

Sources & evidence

ORD record
ord-6240da3860b14ce6844541a2d1475a7f
Source dataset
uspto-grants-2005_06
Patent number
US06902860B2

Reaction notes

Loading…