HuagongsheHuagongshe Chemistry Print Report · For research reference only
Phosphorus sulfide (P2S5) → HCID 86663792, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Phosphorus sulfide (P2S5) | HCID 14817 | — |
| Reactant | Hexamethyldisiloxane | HCID 24764 | — |
| Reactant | HCID 49869278 | HCID 49869278 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 86663792 | HCID 86663792 | 270.7% |
Reaction Steps
A mixture of 3-methyl-4-oxo-N-phenyl-3,4-dihydroimidazo[5,1-d][1,2,3,5]tetrazine-8-carboxamide (430 mg, 1.59 mmol), phosphorus pentasulfide (212 mg, 0.48 mmol) and hexamethyldisiloxane (680 μL, 3.18 mmol) in DCM (20 mL) was refluxed overnight. The crude product was absorbed on silica and was purified by flash chromatography using a gradient elution of DCM:MeOH (100:0 to 98:2) to give 372 mg of 3-methyl-4-oxo-N-phenyl-3,4-dihydroimidazo[5,1-d][1,2,3,5]tetrazine-8-carbothioamide as a 1.5:1 inseparable mixture with the starting material.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09024018B2 |
| Source dataset | uspto-grants-2015_05 |
| ORD ID | ord-68770f884d1f4ec9b678718ff4dc0597 |
| Source note | uspto-grants-2015_05 |