HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanol → HCID 178507925, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | Cesium carbonate | HCID 10796 | — |
| Reactant | 2,4-Diamino-6-chloropyrimidine | HCID 67432 | — |
| Reactant | HCID 178515914 | HCID 178515914 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 178507925 | HCID 178507925 | — |
Reaction Steps
4-(5-{[3-(trifluoromethyl)phenyl]amino}-4H-1,2,4-triazol-3-yl)phenol (160 mg, 0.5 mmol) was dissolved in 3 mL of anhydrous dioxane in 2-5 mL microwave vial (Personal Chemistry). Solid Cs2CO3 (163.0 mg, 0.5 mmol) was added, followed by 4-chloro-2,6,-diaminopyrimidine (79.5 mg, 0.55 mmol). The vial was capped and microwaved at 200° C. for 20 min. Then ca. 3 mL of MeOH was added to dissolve the formed suspension, the solution was transferred into a round-bottom flask and solvent was removed in vacuo. The residue was re-dissolved in 3 mL of DMF, filtered through 0.22 u syringe filter and purified by reverse phase preparative HPLC using acetonitrile/water system with 0.01% of TFA.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08372971B2 |
| Source dataset | uspto-grants-2013_02 |
| ORD ID | ord-6d826eb94b3c4361a0b7aeef62e2e455 |
| Source note | uspto-grants-2013_02 |