HuagongsheHuagongshe Chemistry Print Report · For research reference only
Potassium Carbonate → HCID 58506477, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | 7-hydroxy-2,2-dimethyl-4H-benzo[d][1,3]dioxin-4-one | HCID 10583950 | — |
| Reactant | HCID 11076628 | HCID 11076628 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | HCID 58506477 | HCID 58506477 | 74.2% |
Reaction Steps
A solution of 7-hydroxy-2,2-dimethyl-4H-benzo[d][1,3]dioxin-4-one, (19.4 g, 100 mmol), 2-(2-methoxyethoxy)ethyl 4-methylbenzenesulfonate (27.4 g, 100 mmol) and K2CO3 (41 g, 300 mmol) in CH3CN (500 mL) was refluxed for 4.5 hours. The mixture was poured in H2O (1000 mL) and extracted twice with CH2Cl2 (500 mL). The combined organic layers were washed with brine (100 mL), dried over MgSO4, filtered and concentrated under reduced pressure. The crude product was purified by flash chromatography (PE/EtOAc=9/1) to give the title compound (22 g) as white solid. LC-MS (ES, m/z): 297 [M+H]+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09045440B2 |
| Source dataset | uspto-grants-2015_06 |
| ORD ID | ord-e25fa1284d644f03bfe4e53ad0641e4b |
| Source note | uspto-grants-2015_06 |