Acetic Acid → HCID 89494514, compound

HRID 595067Notes

Reaction equation

HRID 595067 reaction equation
C(S[C:4]1[NH:5][C:6](=[O:14])[C:7]2[CH2:12][S:11][CH:10]([CH3:13])[C:8]=2[N:9]=1)C.Cl.CC(O)=[O:18]>O>[CH3:13][CH:10]1[C:8]2[NH:9][C:4](=[O:18])[NH:5][C:6](=[O:14])[C:7]=2[CH2:12][S:11]1

Participants

5

Reactant 3

HCID 176Acetic AcidHCID 313Hydrochloric AcidHCID 1365978485719-25-5

Product 1

HCID 89494514HCID 89494514, compoundYield 80%

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Procedure

To a suspension of 2-(ethylthio)-7-methylthieno[3,4-d]pyrimidin-4(3H,5H,7H)-one (3.96 g, 17.3 mmol) in water (20 mL) was added 2.0 mL of conc. HCl and 4.0 mL of AcOH. The mixture was heated to reflux overnight then cooled and the precipitated solid collected by filtration, washed with water and methanol, evaporated and dried to obtain 7-methylthieno[3,4-d]pyrimidine-2,4(1H,3H,5H,7H)-dione as a white solid (2.52 g, 80%). Without further purification, the crude product was used directly in the next step.

Workup

  1. temperatureThe mixture was heated
  2. temperatureto reflux overnight
  3. temperaturethen cooled
  4. filtrationthe precipitated solid collected by filtration
  5. washwashed with water and methanol
  6. customevaporated
  7. customdried

Sources & evidence

ORD record
ord-0a4dc8363f3044749f2618383848e550
Source dataset
uspto-grants-2016_01
Patent number
US09242993B2

Reaction notes

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