HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methane → HCID 178477337, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methane | HCID 297 | — |
| Reactant | Pyridine | HCID 1049 | — |
| Reactant | Phosphorus sulfide (P2S5) | HCID 14817 | — |
| Reactant | NSC403089 | HCID 135424359 | — |
| Solvent | Sodium Hydroxide | HCID 14798 | — |
| Product | HCID 178477337 | HCID 178477337 | 95.9% |
Reaction Steps
A mixture of 4-oxo-7-ethylthio-3H-pyrimido[4,5-d]pyrimidine (1.33 g, 6.7 mmol), P2S5 (1.48 g, 6.6 mmol) and pyridine (15 mL) is refluxed under N2 for 3 h. The pyridine is then stripped under reduced pressure, and the residue is dissolved in NaOH solution (0.5 M, 75 mL) and boiled with charcoal. After filtration, the filtrate is neutralized with acetic acid to generate a gold brown solid. Buchner filtration and drying in a vacuum oven affords 4-thiono-7-ethylthio-3H-pyrimido[4, 5-d]pyrimidine (1.42 g, 95%). 1H NMR (DMSO) δ 9.47 (1H, s), 8.46 (1H, s), 3.20 (2H, q, J=7.3 Hz), 1.35 (3H, t, J=7.3 Hz).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06713484B2 |
| Source dataset | uspto-grants-2004_03 |
| ORD ID | ord-13a78056ba6c4d18977d615e79a53225 |
| Source note | uspto-grants-2004_03 |