HuagongsheHuagongshe Chemistry Print Report · For research reference only
Potassium Carbonate → HCID 11189483, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | 4,5-Dichlorocatechol | HCID 18909 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | tert-Butyl bromoacetate | HCID 79177 | — |
| Reactant | 2-Chloro-1-fluoro-4-methylsulfonylbenzene | HCID 21340880 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 11189483 | HCID 11189483 | — |
Reaction Steps
A mixture of sodium hydride (60% wt. disp. in oil, 0.223 g) and 4,5-dichlorocatechol (1 g) in DMF (10 ml) was stirred at RT for 15 min. tert-Butyl-bromoacetate (0.9 ml) was added, stirred at RT for 2 h then potassium carbonate (0.77 g) and the product from example 7 step (ii) (0.7 g) added and the mixture heated at 90° C. for 14 h. The mixture was partitioned between 2M sodium hydroxide solution and diethylether, the aqueous layer was acidified with 2M hydrochloric acid and extracted with ethylacetate. The ethylacetate layer was dried, evaporated under reduced pressure and the residue purified by RPHPLC. Yield 0.349 g.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08003703B2 |
| Source dataset | uspto-grants-2011_08 |
| ORD ID | ord-ece191b7d1d443b69da755976e4a3af5 |
| Source note | uspto-grants-2011_08 |