Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydrogen Bromide | HCID 260 | — |
| Reactant | HCID 18385121 | HCID 18385121 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Product | HCID 18385099 | HCID 18385099 | 97% |
Reaction Steps
In a flask was added the compound obtained in Example 1, (1.0 g, 2.36 mmol) in acetic acid (30 mL). To this solution was added hydrobromic acid (33% in acetic acid, 8 mL), and the flask was sealed. The flask was heated with stirring in an oil bath (80° C.) for 12 hours. The reaction was monitored on LC-MS, which confirmed the completion of the reaction. The volatiles were removed in vaccuo, and the residue was partitioned between ethyl acetate and water (50+50 mL). The organic phase was washed twice with water and once with brine and evaporated to give a 1.1 g (97%) of the title compound as a crude product, pure enough to be used further without purification.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06492406B1 |
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| Source dataset | uspto-grants-2002_12 |
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| ORD ID | ord-3eb797f0639c4614999a0a9273a35c7c |
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| Source note | uspto-grants-2002_12 |
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