HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dimethyl Sulfate → HCID 9847767, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dimethyl Sulfate | HCID 6497 | — |
| Reactant | Ethyl Acetate | HCID 8857 | — |
| Reactant | Potassium Hydroxide | HCID 14797 | — |
| Reactant | HCID 22339706 | HCID 22339706 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 9847767 | HCID 9847767 | — |
Reaction Steps
To a stirred solution of 2-{4-[3-(4-fluoro-benzoyl)-4-methoxy-phenoxy]-3,5-dimethyl-phenyl}-2H-[1,2,4]triazine-3,5-dione (50 mg) and potassium hydroxide (12 mg) in methanol (2 mL) was added dimethylsulfate (41 mg) to produce a thick slurry. After 3 h, the reaction mixture was diluted into ethyl acetate, washed with 1N aqueous sodium hydroxide, the organic layer dried over sodium sulfate, filtered and concentrated in vacuo. The resulting oil was flash chromatographed on silica gel (20%-35% ethyl acetate/hexanes) to afford the title compound of this EXAMPLE as a colorless solid, 24 mg. MS Calc.:475.5 Found:476.2 (M+1).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06787652B1 |
| Source dataset | uspto-grants-2004_09 |
| ORD ID | ord-06c9ebb586f34baab3a34e998c570a5c |
| Source note | uspto-grants-2004_09 |