HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dimethylhydantoin → HCID 22351160, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dimethylhydantoin | HCID 6491 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | 1-Naphthalenesulfonyl chloride | HCID 66560 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 22351160 | HCID 22351160 | 6% |
Reaction Steps
5,5-Dimethylimidazolidine-2,4-dione (1.28 g) was dissolved in tetrahydrofuran (20 mL), and sodium hydride (60%, in oil) (0.25 g) was added at 0° C. under ice-cooling. After stirred for 30 minutes, 1-naphthalenesulfonyl chloride (2.38 g) was added at 0° C., and the mixture was stirred at room temperature overnight. After the solvent was distilled off, ethyl acetate (150 mL) was added to the reaction solution, and the mixture was washed with 1N hydrochloric acid, an aqueous saturated sodium bicarbonate solution and a saturated brine in turn. After drying over anhydrous magnesium sulfate, the solvent was distilled off. Further purification by silica gel chromatography (hexane:ethyl acetate=2:1) afforded 160 mg of white crystals.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06919365B2 |
| Source dataset | uspto-grants-2005_07 |
| ORD ID | ord-e63c587fb0c64115a894a1782ce89a65 |
| Source note | uspto-grants-2005_07 |