Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Bromine | HCID 24408 | — |
| Reactant | HCID 86723526 | HCID 86723526 | — |
| Solvent | Chloroform | HCID 6212 | — |
| Product | HCID 86723528 | HCID 86723528 | — |
Reaction Steps
5-Benzoyl-1,3-diethyl-6-methylpyrimidine-2,4(1H,3H)-dione (step 2)(800 mg, 2.79 mmol) was dissolved in chloroform (Volume: 60 mL) and bromine (0.288 mL, 5.59 mmol) was added. The mixture was heated at 60° C. for 1 h. A further portion of bromine (0.288 mL, 5.59 mmol) was added. The mixture was heated for 30 mins and further bromine (0.288 mL, 5.59 mmol) was added. The reaction mixture was cooled to RT and washed with aqueous sodium metabisulfite. The organic phase was separated, passed through a hydrophobic frit and evaporated under vacuum. The residue was dissolved in DCM and evaporated onto silica. The silica was deposited onto a 10 g silica cartridge and the system eluted with 20% EtOAc/hexane, 30% EtOAc/hexane, and 40% EtOAc/hexane.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US09359381B2 |
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| Source dataset | uspto-grants-2016_06 |
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| ORD ID | ord-c3d8a37a759141319289b6404ba07f99 |
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| Source note | uspto-grants-2016_06 |
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