HuagongsheHuagongshe Chemistry Print Report · For research reference only
Calcium Carbonate → 6-fluoro-3H-isobenzofuran-1-one
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Calcium Carbonate | HCID 10112 | — |
| Reactant | Methyl 2-(bromomethyl)-5-fluorobenzoate | HCID 15155455 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | 6-fluoro-3H-isobenzofuran-1-one | HCID 11171082 | 92% |
Reaction Steps
A mixture of methyl 2-(bromomethyl)-5-fluorobenzoate (0.750 g, 3.04 mmol) and calcium carbonate (1.823 g, 18.21 mmol) in 1,4-dioxane (30 mL) and water (30.0 mL) was heated at reflux for 2.5 hr. The insoluble material was removed by filtration. The filtrate was concentrated under vacuum and then extracted with CH2Cl2 (4×30 mL). The combined extract was dried over anhydrous MgSO4. Removal of solvent under vacuum provided the desired product (0.423 g, 2.78 mmol, 92% yield) as a white solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08685969B2 |
| Source dataset | uspto-grants-2014_04 |
| ORD ID | ord-1d39b7fe63c14925a9f9c1401874f7d7 |
| Source note | uspto-grants-2014_04 |