Formic Acid → HCID 9815972, compound

HRID 883558Notes

Reaction equation

HRID 883558 reaction equation
[NH2:1][C:2]1[C:3](=[O:14])[NH:4][C:5](=[S:13])[N:6]([CH2:9][CH2:10][O:11][CH3:12])[C:7]=1[NH2:8].[CH:15](O)=O>>[CH3:12][O:11][CH2:10][CH2:9][N:6]1[C:7]2[N:8]=[CH:15][NH:1][C:2]=2[C:3](=[O:14])[NH:4][C:5]1=[S:13]

Participants

3

Reactant 2

HCID 284Formic AcidHCID 86601061HCID 86601061, compound

Product 1

HCID 9815972HCID 9815972, compound

Conditions

Temperature
90 °C

Procedure

5,6-Diamino-1-(2-methoxy-ethyl)-2-thioxo-2,3-dihydro-1H-pyrimidin-4-one (0.27 g, 1.3 mmol) was suspended in formic acid (2 mL) and this solution was heated at 90° C. for 1.5 h. Excess formic acid was evaporated off under reduced pressure. 10% Sodium hydroxide solution (5 mL) was added to the orange solid and the resulting solution was heated at 90° C. for 2 h. The reaction mixture was neutralized with dilute acetic acid. The resulting solution was put in the fridge for several days, then the orange needle-like crystals that had formed were collected by filtration and washed with water. Yield: (0.11 g, 40%).

Workup

  1. customExcess formic acid was evaporated off under reduced pressure
  2. addition10% Sodium hydroxide solution (5 mL) was added to the orange solid
  3. temperaturethe resulting solution was heated at 90° C. for 2 h
  4. waitThe resulting solution was put in the fridge for several days
  5. customthe orange needle-like crystals that had formed
  6. filtrationwere collected by filtration
  7. washwashed with water

Sources & evidence

ORD record
ord-32ff7b1227b04d5aa58ce49cf802ef2d
Source dataset
uspto-grants-2012_08
Patent number
US08236951B2

Reaction notes

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