HuagongsheHuagongshe Chemistry Print Report · For research reference only
Urea → Thieno(3,2-d)pyrimidine-2,4(1H,3H)-dione
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Urea | HCID 1176 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | Methyl 3-amino-2-thiophenecarboxylate | HCID 89652 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | Thieno(3,2-d)pyrimidine-2,4(1H,3H)-dione | HCID 7059273 | 61.5% |
Reaction Conditions
| Temperature | 190 °C |
|---|
Reaction Steps
Methyl 3-aminothiophene-2-carboxylate (4.9 g, 31.3 mmol) and urea (19 g, 187 mmol) were dissolved in N,N-dimethylformamide (10 mL), the reaction temperature was raised to 190° C., followed by stirring for 12 hours. After the reaction was complete, the reaction mixture was added to 1N NaOH aqueous solution, cooled to room temperature and filtered under a reduced pressure to remove the insoluble precipitate. The filtrate was acidified (pH 2) with 2N HCl aqueous solution, and the resulting solid was filtered under a reduced pressure with washing using distilled water. The resulting solid was dried under a reduced pressure to obtain the title compound (yield: 3.2 g, 61.5%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08957065B2 |
| Source dataset | uspto-grants-2015_02 |
| ORD ID | ord-36b993d08b2246cdaaa83ca3fabaf76a |
| Source note | uspto-grants-2015_02 |