HuagongsheHuagongshe Chemistry Print Report · For research reference only
Lithium borohydride → 3,8-dibromo-6H-benzo[c]chromene
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Lithium borohydride | HCID 4148881 | — |
| Reactant | 3,8-Dibromo-benzo[c]chromen-6-one | HCID 59561042 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | 3,8-dibromo-6H-benzo[c]chromene | HCID 59610756 | 86% |
Reaction Steps
To a solution of 3,8-dibromo-benzo[c]chromen-6-one (650 mg, 1.85 mmol) in THF (20 mL) was added 2 M solution of LiBH4 in THF (3.7 mL, 7.4 mmol). The mixture was stirred for 3 hours at room temperature. Quenched slowly with ammonium chloride solution. The mixture was extracted with ethyl acetate, dried over Na2SO4, filtered and concentrated in vacuo. The obtained residue was suspended in 85% phosphoric acid (20 mL) and heated at 160° C. for 4 h. The mixture was extracted with ethyl acetate, washed with water, dried over Na2SO4, filtered and concentrated in vacuo. The obtained residue was purified by flash chromatography to provide the desired product 3,8-Dibromo-6H-benzo[c]chromene as a white solid (539 mg, 86%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08841278B2 |
| Source dataset | uspto-grants-2014_09 |
| ORD ID | ord-2b82d37bdc344eaea0b16716bb7e4102 |
| Source note | uspto-grants-2014_09 |