HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Carbonate → 7-Chloro-5-methyl-2-(1-methylethyl)[1,2,4]triazolo[1,5-a]pyrimidine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Carbonate | HCID 10340 | — |
| Reactant | Phosphorus oxychloride | HCID 24813 | — |
| Reactant | HCID 178429167 | HCID 178429167 | — |
| Solvent | Water | HCID 962 | — |
| Product | 7-Chloro-5-methyl-2-(1-methylethyl)[1,2,4]triazolo[1,5-a]pyrimidine | HCID 53391863 | — |
Reaction Steps
A suspension of Intermediate 17 (0.225 g, 1.171 mmol) in phosphorous oxychloride (ALDRICH, 0.327 ml, 3.51 mmol) was heated under reflux for 1 h. The reaction mixture was added dropwise into iced water, neutralized with solid Na2CO3 and product was extracted with DCM. The combined organic layers were washed with brine and dried over anhydrous Na2SO4. A brown oil was obtained upon solvent removal in vacuo which was purified by flash chromatography (Si, eluting with Hexane:EtOAc mixtures from 100:0 to 40:60%) to yield the title compound as a white solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09238653B2 |
| Source dataset | uspto-grants-2016_01 |
| ORD ID | ord-36824fea01cc4572a3716e4a9506d30b |
| Source note | uspto-grants-2016_01 |