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HuagongsheHuagongshe Chemistry Print Report · For research reference only
HRID 1059636Generated: October 29, 2026

Methane → HCID 178477337, compound

https://huagongshe.com/reaction/1059636

Reaction equation

Participants

RoleNameHCIDCharge
ReactantMethaneHCID 297—
ReactantPyridineHCID 1049—
ReactantPhosphorus sulfide (P2S5)HCID 14817—
ReactantNSC403089HCID 135424359—
SolventSodium HydroxideHCID 14798—
ProductHCID 178477337HCID 17847733795.9%

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

DOI10.6084/m9.figshare.5104873.v1
Patent numberUS06521620B1
Source datasetuspto-grants-2003_02
ORD IDord-2a76675422fe4a04bbb03d96e8f50407
Source noteuspto-grants-2003_02