HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methyl iodide → HCID 24850584, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methyl iodide | HCID 6328 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | Dichloromethane methanol | HCID 21226129 | — |
| Reactant | HCID 59803672 | HCID 59803672 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 24850584 | HCID 24850584 | — |
Reaction Steps
A mixture of 2.0 g (5.3 mmol) of 8-(3,4-dimethoxyphenylethynyl)-3-ethyl-1-prop-2-ynyl-3,7-dihydropurine-2,6-dione, potassium carbonate (0.83 g, 6 mmol) and methyl iodide (0.6 ml, 10 mmol) in dimethylformamide (20 ml) was stirred at room temperature for 0.5 h (TLC-control: dichloromethane/methanol, 9.5:0.5). The product was precipitated by addition of water (100 ml), filtered under reduced pressure, was washed with water and dried at 70° C. Further purification was achieved by column chromatography on silica gel (eluent: dichloromethane/methanol, 9.5:0.5) and subsequent crystallization from dichloromethane/petroleum ether. Yield: 1.76 g, 80% (crude product); m.p.: 221.5° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08044061B2 |
| Source dataset | uspto-grants-2011_10 |
| ORD ID | ord-63e6af4a999b486083cc5f906d96f025 |
| Source note | uspto-grants-2011_10 |