HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 46945966, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Dimethylhydantoin | HCID 6491 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | 5-Fluoro-2-nitrotoluene | HCID 94956 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 46945966 | HCID 46945966 | 25% |
Reaction Steps
A mixture of 5-fluoro-2-nitrotoluene (1.55 g, 10 mmoles), 5,5-dimethylhydantoin (1.28 g, 10 mmoles), K2CO3 (1.38 g, 10 mmoles) in DMF (15 ml) is introduced into a vial intended to be placed in a microwave oven and irradiated at 100° C. for 70 minutes, under magnetic stirring. The reaction mixture is then poured into water (200 ml) and extracted with AcOEt (2×75 ml). The organic phases are combined, washed with salt water, dried over Na2SO4 and filtered. The filtrate is concentrated under reduced pressure and the residue is purified by chromatography on a silica column (eluent: Heptane/AcOEt:7/3). The expected compound is obtained in the form of a white solid with a yield of 25% (666 mg). Melting point: 177-178° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08710091B2 |
| Source dataset | uspto-grants-2014_04 |
| ORD ID | ord-70d82c744e5f48ca9d940dffe9b79d75 |
| Source note | uspto-grants-2014_04 |