HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 59496108, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Water | HCID 962 | — |
| Reactant | Pyridine | HCID 1049 | — |
| Reactant | Benzoyl chloride | HCID 7412 | — |
| Reactant | HCID 59496098 | HCID 59496098 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 59496108 | HCID 59496108 | 16.3% |
Reaction Steps
Benzoyl chloride (0.253 ml, 2.180 mmol) was added to a solution of 2-acetyl-6-phenyl-1,2,4-triazine-3,5(2H,4H)-dione (420 mg, 1.817 mmol) and pyridine (0.441 ml, 5.45 mmol) in 1,4-Dioxane (5 ml) at 5° C. Mixture was stirred at r.t. overnight. Solids were filtered off and rinsed with DCM, solvent was concentrated under reduced pressure. Residue was diluted in ethanol (20 ml), hydrochloric acid 37% in water (0.250 ml, 3.04 mmol) was added and mixture heated at 90° C. for 3 h. Solvent was concentrated and residue purified on biotage 25M silica cartridge, eluting with Cy/AcOEt 8:2 to AcOEt 100%, to give 87 mg of title compound (16% yield).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08217168B2 |
| Source dataset | uspto-grants-2012_07 |
| ORD ID | ord-3717e946e0dd4f0884b321665d19f535 |
| Source note | uspto-grants-2012_07 |