HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 58566366, compound → 5-chloro-7-(hydroxymethyl)-2,2-dimethylbenzofuran-3(2H)-one
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 58566366 | HCID 58566366 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | 5-chloro-7-(hydroxymethyl)-2,2-dimethylbenzofuran-3(2H)-one | HCID 58566578 | 11% |
Reaction Steps
To a solution of 5-chloro-2,2-dimethyl-3-oxo-2,3-dihydrobenzofuran-7-carboxylic acid (655) (2.67 g, 11.1 mmol) in tetrahydrofuran (56 mL) was added BH3.tetrahydrofuran (11.1 mL, 11.1 mmol) drop wise and stirred overnight. The reaction was quenched with water and methanol and then extracted with ethyl acetate. The organic layer was washed with saturated sodium bicarbonate and then dried over sodium sulfate, filtered and concentrated in vacuo. The crude compound was purified by flash column chromatography on silica gel with hexanes and EtOAc (50%) to afford 5-chloro-7-(hydroxymethyl)-2,2-dimethylbenzofuran-3(2H)-one (656) (278 mg). The saturated sodium bicarbonate layer was acidified to recover the starting acid (655) (1.68 g).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08299117B2 |
| Source dataset | uspto-grants-2012_10 |
| ORD ID | ord-82e3dcb3a35d4b3889022407b6f46f1f |
| Source note | uspto-grants-2012_10 |