HuagongsheHuagongshe Chemistry Print Report · For research reference only
Cesium carbonate → HCID 23447918, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Cesium carbonate | HCID 10796 | — |
| Reactant | Ethanol, 2,2,2-trifluoro-, 1-(4-methylbenzenesulfonate) | HCID 67942 | — |
| Reactant | HCID 23447878 | HCID 23447878 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | HCID 23447918 | HCID 23447918 | 52% |
Reaction Steps
A stirred mixture of 2.83 g of Compound 4A, 6.05 g of cesium carbonate and 2.95 g of 2,2,2-trifluoroethyl p-toluenesulphonate in 60 mL of acetonitrile was refluxed for 16 hours. The solvent was evaporated at reduced pressure. 90 mL of brine was added to the residue and the mixture was extracted with 3×40 mL of ethyl acetate. The organic layer was washed with 3×20 mL of water and 20 mL of brine, and dried over sodium sulphate. The solvent was removed at reduced pressure and the residue purified by flash chromatography (petroleum ether/ethyl acetate gradient 95:5 to 80:20). The solvents were removed in vacuo to give 1.86 g (52%) of Compound 4B as a white solid. M.p. (98) 102-105° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06680319B2 |
| Source dataset | uspto-grants-2004_01 |
| ORD ID | ord-8839cd1c55894e8b9813ea2c915a8e79 |
| Source note | uspto-grants-2004_01 |