HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dimethyl Sulfate → HCID 131736982, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dimethyl Sulfate | HCID 6497 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | HCID 131736981 | HCID 131736981 | — |
| Solvent | Acetone | HCID 180 | — |
| Product | HCID 131736982 | HCID 131736982 | 19% |
Reaction Steps
To a solution of tert-butyl (6-((tert-butoxycarbonyl)(4-(hydroxymethyl)-2-nitrophenyl)amino)pyrimidin-4-yl)(methyl)carbamate (1.5 g, 3.488 mmol) in acetone (20 mL) under an argon atmosphere at 0° C., was added potassium carbonate (0.48 g, 6.97 mmol) followed by dimethyl sulfate (0.87 g, 6.97 mmol). The resulting reaction mixture was then refluxed for 24 h and then allowed to cool to rt. The reaction mixture was concentrated under vacuum to obtain a crude residue. The residue was purified by silica gel column chromatography to afford the title compound (0.3 g, yield: 19%) as a solid. MS (ESI): 490.55 [M+H]+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09434697B2 |
| Source dataset | uspto-grants-2016_09 |
| ORD ID | ord-48e3532d41394c3f97f034e26bd5c398 |
| Source note | uspto-grants-2016_09 |