HuagongsheHuagongshe Chemistry Print Report · For research reference only
Potassium Carbonate → HCID 86605564, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | 1-Chloropinacolone | HCID 83572 | — |
| Reactant | HCID 86605563 | HCID 86605563 | — |
| Solvent | Methyl Ethyl Ketone | HCID 6569 | — |
| Product | HCID 86605564 | HCID 86605564 | 108.2% |
Reaction Steps
To a solution of 5-[1-ethyl-1-(4-hydroxy-3-methyl-phenyl)-propyl]-3-methyl-thiophene-2-sulfonic acid dimethylaminemethyleneamide (5.1 g, 12.48 mmol) in 2-butanone (50 ml) is added potassium carbonate (2.59 g, 18.72 mmol), and chloropinacolone (3.28 ml, 24.91 mmol). The reaction is refluxed overnight, filtered, and concentrated. The residue is partitioned between EtOAc (400 ml) and 0.2N HCl (100 ml). The organic layer is washed with brine (100 ml), MgSO4 dried, concentrated, and chromatographed (120 g SiO2, 50% EtOAc/Hex) to yield the title compound (6.11 g, 97%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07601850B2 |
| Source dataset | uspto-grants-2009_10 |
| ORD ID | ord-312a0c4b33e7472b922c270c7d0d28b1 |
| Source note | uspto-grants-2009_10 |