HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Hydroxide → 5H-pyrimido-[4,5-b][1,4]oxazin-6-one
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | Tin tetrachloride | HCID 24287 | — |
| Reactant | (6-Chloro-5-nitro-pyrimidin-4-yloxy)-acetic acid methyl ester | HCID 86650561 | — |
| Solvent | Hydrochloric Acid | HCID 313 | — |
| Product | 5H-pyrimido-[4,5-b][1,4]oxazin-6-one | HCID 53790813 | — |
Reaction Steps
In a 25 ml flask, (6-chloro-5-nitro-pyrimidin-4-yloxy)-acetic acid methyl ester (280 mg, 1.1 mmol) and tin tetrachloride (849 mg, 4.5 mmol) were dissolved in hydrochloric acid (7 ml) and heated for 1 hour at 80□. The reaction mixture was cooled to room temperature and neutralized by adding 10% sodium hydroxide solution dropwise, and the formed solid was removed by filtration. The filtrate was extracted with ethyl acetate, and the combined organic layer was washed with saturated saline solution, dried over anhydrous sodium sulfate (Na2SO4), filtered and evaporated under reduced pressure. The obtained yellow solid mixture (107 mg) was used in the next step without further purification.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08394792B2 |
| Source dataset | uspto-grants-2013_03 |
| ORD ID | ord-ad2488066abb447b94dc739b108706b8 |
| Source note | uspto-grants-2013_03 |