HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sulfuric Acid → Ethyl 7-bromo-4-hydroxy-1,1-dimethyl-2-oxo-naphthalene-3-carboxylate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sulfuric Acid | HCID 1118 | — |
| Reactant | Phosphorus oxide (P4O10) | HCID 14812 | — |
| Reactant | Diethyl 2-(2-(3-bromophenyl)-2-methylpropanoyl)malonate | HCID 67099417 | — |
| Product | Ethyl 7-bromo-4-hydroxy-1,1-dimethyl-2-oxo-naphthalene-3-carboxylate | HCID 67099405 | 41.1% |
Reaction Steps
H2SO4 (60 mL, 710 mmol) was cooled to 0° C. and treated with P2O5 (20 g, 141 mmol). The mixture was brought to room temperature and added to diethyl 2-(2-(3-bromophenyl)-2-methylpropanoyl)malonate (17.44 g, 45 mmol). The reaction mixture was then stirred for 2 hours. Ice (H2O) was added, and the aqueous mixture was extracted with EtOAc (3×). The combined organic layers were washed with water (2×) and brine, dried (MgSO4), and concentrated in vacuo to give the crude compound as an orange oil. The crude oil was purified by silica flash chromatography (0-100% DCM/hexane) to give the desired compound as a white solid (6.27 g). MS (m/e)=339.1 (M+H)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07928139B2 |
| Source dataset | uspto-grants-2011_04 |
| ORD ID | ord-1e44710e04044b1e969640f9878ee47b |
| Source note | uspto-grants-2011_04 |