HuagongsheHuagongshe Chemistry Print Report · For research reference only
Potassium Carbonate → [7-(2-Butynyl)-1-methyl-2,6-dioxo-1,2,6,7-tetrahydropurin-3-yl]methyl 2,2-dimethylpropionate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | 1-Bromo-2-butyne | HCID 2756862 | — |
| Reactant | [1-Methyl-2,6-dioxo-1,2,6,7-tetrahydropurin-3-yl]methyl 2,2-dimethylpropionate | HCID 23536866 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | [7-(2-Butynyl)-1-methyl-2,6-dioxo-1,2,6,7-tetrahydropurin-3-yl]methyl 2,2-dimethylpropionate | HCID 23536882 | — |
Reaction Steps
2,2-Dimethylpropionic acid [1-methyl-2,6-dioxo-1,2,6,7-tetrahydropurin-3-yl]methyl ester (1.871 g) was dissolved in N,N-dimethylformamide (30 ml), potassium carbonate (1.5 g) and 2-butynyl bromide (0.7 ml) were added to the solution, and the mixture was stirred at room temperature overnight. The reaction mixture was diluted with ethyl acetate, and washed with water and 1N hydrochloric acid. The organic layer was dried over anhydrous magnesium sulfate and filtered. Then, the solvent was removed by distillation. The residue was purified by silica gel column chromatography to give 2.12 g of the title compound from the elution fraction of hexane-ethyl acetate (3:2).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07074798B2 |
| Source dataset | uspto-grants-2006_07 |
| ORD ID | ord-375bbb219b1e45e280b6eb86b75a52a1 |
| Source note | uspto-grants-2006_07 |