Methanol → HCID 12272877, compound

HRID 1251940Notes

Reaction equation

HRID 1251940 reaction equation
[CH3:1][C:2]1[C:3]([NH2:10])=[N:4][C:5](Cl)=[N:6][C:7]=1Cl.[CH3:11][O-:12].[Na+].[CH3:14][OH:15]>>[NH2:10][C:3]1[C:2]([CH3:1])=[C:7]([O:12][CH3:11])[N:6]=[C:5]([O:15][CH3:14])[N:4]=1

Participants

4

Reactant 3

HCID 887MethanolHCID 10942334Sodium MethoxideHCID 12272880HCID 12272880, compound

Product 1

HCID 12272877HCID 12272877, compoundYield 60%

Procedure

A mixture of 10.7 g (0.06 mol) of 5-methyl-4-amino-2,6-dichloropyrimidine, 100 ml of methanol and 22 g of 30% sodium methylate (0.122 mol) is allowed to react at 120° C. for 20 hours in an autoclave. After cooling, the grey reaction mixture is concentrated in vacuo; the residue is taken up in 70 ml of water, stirred and then filtered. The residue is washed with water, dried and recrystallised from carbon tetrachloride. There remain after drying 6.1 g of 4-amino-5-methyl-2,6-dimethoxypyrimidine as white crystals, which melt at 60° C. (yield=60% of theory).

Workup

  1. customto react at 120° C. for 20 hours in an autoclave
  2. temperatureAfter cooling
  3. concentrationthe grey reaction mixture is concentrated in vacuo
  4. filtrationfiltered
  5. washThe residue is washed with water
  6. customdried
  7. customrecrystallised from carbon tetrachloride
  8. dry with materialafter drying 6.1 g of 4-amino-5-methyl-2,6-dimethoxypyrimidine as white crystals, which
  9. custommelt at 60° C.

Sources & evidence

ORD record
ord-b8c699e19c0d4ed09d82bd426611ad3e
Source dataset
uspto-grants-1988_05
Patent number
US04741760

Reaction notes

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