HuagongsheHuagongshe Chemistry Print Report · For research reference only
Bromine → HCID 68743707, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Bromine | HCID 24408 | — |
| Reactant | N-bromobutanimide | HCID 67184 | — |
| Reactant | HCID 68743754 | HCID 68743754 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | HCID 68743707 | HCID 68743707 | 97.5% |
Reaction Steps
A solution of Intermediate 31 (5.20 g) in acetonitrile (50 ml) was warmed to 35° C., added dropwise with bromine (1.1 ml, WAKO), then added with NBS (3.72 g), and stirred at room temperature for 2 hours. The reaction mixture was concentrated under reduced pressure, then added with ethyl acetate (200 ml), and washed successively with saturated aqueous ammonium chloride, 5% aqueous sodium sulfite, saturated aqueous sodium hydrogencarbonate and saturated brine. The organic layer was dried, and then the solvent was evaporated under reduced pressure. The residue was purified by column chromatography (Quad, hexane:ethyl acetate=10:1) to obtain the title compound (Compound No. E-1, 6.51 g).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07470807B2 |
| Source dataset | uspto-grants-2008_12 |
| ORD ID | ord-2d4e6ba7d9d242e6bebd7806ef775a33 |
| Source note | uspto-grants-2008_12 |