HuagongsheHuagongshe Chemistry Print Report · For research reference only
Potassium Carbonate → 3-[3-(1-Cyclohexylazetidin-3-ylamino)-4-trifluoromethoxyphenyl]-5,5-dimethyl-1-pyridin-4-ylmethyl-imidazolidine-2,4-dione
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | 3-(3-Amino-4-trifluoromethoxyphenyl)5,5-dimethyl-1-pyridin-4-ylmethylimidazolidine-2,4-dione | HCID 23110308 | — |
| Reactant | 1-Cyclohexylazetidin-3-yl methanesulphonate oxalate | HCID 86617226 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | 3-[3-(1-Cyclohexylazetidin-3-ylamino)-4-trifluoromethoxyphenyl]-5,5-dimethyl-1-pyridin-4-ylmethyl-imidazolidine-2,4-dione | HCID 66915811 | — |
Reaction Steps
300 mg (0.76 mmol) of 3-(3-amino-4-trifluoromethoxyphenyl)5,5-dimethyl-1-pyridin-4-ylmethylimidazolidine-2,4-dione were dissolved in 15 ml of ethyl acetate, admixed with 492 mg (1.52 mmol) of 1-cyclohexylazetidin-3-yl methanesulphonate oxalate and 631 mg (4.56 mmol) of K2CO3, and heated under reflux for 4 h. To complete the reaction, a further 49 mg (0.15 mmol) of 1-cyclohexylazetidin-3-yl methanesulphonate oxalate and 63 mg (0.46 mmol) of K2CO3 were added, and the mixture was stirred under reflux once again for 2 h. Subsequently, the mixture was concentrated and the residue purified by flash chromatography (150 g of silica gel/95:5 CH2C12:CH3OH).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07759379B2 |
| Source dataset | uspto-grants-2010_07 |
| ORD ID | ord-0c29a66265eb4608b6f0e8e20dca3194 |
| Source note | uspto-grants-2010_07 |