Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Bromine | HCID 24408 | — |
| Reactant | HCID 23116895 | HCID 23116895 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Product | HCID 87181622 | HCID 87181622 | 62% |
Reaction Steps
While cooling acetic acid solution prepared by dissolving 25 g (160.1 mmol) of 2,4-difluorophenyl acetophenone in an amount of 50 milliliter down to 10° C. or cooler, 25.5 g (160.1 mmol) of bromine was dripped and the resultant solution reacted for 7 hours. Throwing the resultant solution into 300 milliliter of water, the solution was extracted with the use of methylene chloride. After drying an organic layer with the use of magnesium sulfide, the solvent was removed. Refining the resultant residues by means of silica column (hexane), 23.4 g of α-bromo-2,4-difluorophenyl acetophenone Intermediate 1-2c as brown oil was obtained (yield: 62%). The brown oil was confirmed as the aimed compound from 1H-NMR spectrum. The measurement result is shown as follows:
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08106390B2 |
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| Source dataset | uspto-grants-2012_01 |
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| ORD ID | ord-41a125d509e34760b9de8951c8476f8e |
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| Source note | uspto-grants-2012_01 |
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