Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Bromine | HCID 24408 | — |
| Reactant | HCID 10944431 | HCID 10944431 | — |
| Catalyst | Tungsten | HCID 23964 | — |
| Solvent | Chloroform | HCID 6212 | — |
| Product | HCID 11723190 | HCID 11723190 | 50.2% |
Reaction Steps
A solution of ethyl 2-[2-(ethyloxy)-2-oxoethyl]benzoate (4.15 g, 17.5 mmol) in chloroform (70 ml) was treated with bromine (1.3 ml, 25 mmol) and stirred at reflux, whilst irradiating with a 120 W tungsten bulb, for 5 hrs. The mixture was cooled to 20° C., evaporated and purified by automated flash silica-gel column chromatography (using a Biotage SP4), eluting with 0-10% gradient of ethyl acetate in hexane (10 column volumes), to give ethyl 2-[1-bromo-2-(ethyloxy)-2-oxoethyl]benzoate (2.77 g) as a pale yellow oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07935832B2 |
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| Source dataset | uspto-grants-2011_05 |
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| ORD ID | ord-d7d4128c3d9048e0987d805837c91250 |
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| Source note | uspto-grants-2011_05 |
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