Formic Acid → HCID 13050739, compound

HRID 1632478Notes

Reaction equation

HRID 1632478 reaction equation
[NH2:1][C:2]1[C:3]([N:10]([CH2:13][CH3:14])[CH2:11][CH3:12])=[N:4][C:5]([CH3:9])=[N:6][C:7]=1[SH:8].[CH:15](O)=O>>[CH2:13]([N:10]([CH2:11][CH3:12])[C:3]1[C:2]2[N:1]=[CH:15][S:8][C:7]=2[N:6]=[C:5]([CH3:9])[N:4]=1)[CH3:14]

Participants

3

Reactant 2

HCID 284Formic Acid2×HCID 178463880HCID 178463880, compound

Product 1

HCID 13050739HCID 13050739, compound

Procedure

3 g of 5-amino-4-diethylamino-6-mercapto-2-methylpyrimidine was dissolved in 50 ml of 90% formic acid and refluxed for 2 hours. After the completion of the reaction, formic acid was distilled off under reduced pressure. The residue was added with 30 ml of water, and neutralized with ammonium hydroxide. This aqueous solution was extracted with 200 ml of ethyl acetate and the organic layer was dried over sodium sulphate anhydride. Then the solvent was distilled off under reduced pressure, and the residue was purified by column chromatography on silica-gel to obtain 7-diethylamino-5-methylthiazolo[5,4-d]pyrimidine (1.6 g).

Workup

  1. temperaturerefluxed for 2 hours
  2. distillationwas distilled off under reduced pressure
  3. additionThe residue was added with 30 ml of water
  4. extractionThis aqueous solution was extracted with 200 ml of ethyl acetate
  5. dry with materialthe organic layer was dried over sodium sulphate anhydride
  6. distillationThen the solvent was distilled off under reduced pressure
  7. customthe residue was purified by column chromatography on silica-gel

Sources & evidence

ORD record
ord-16aa9949d73c4285a60f3e909bbb9138
Source dataset
uspto-grants-1984_10
Patent number
US04476127

Reaction notes

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