Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Bromine | HCID 24408 | — |
| Reactant | Sodium Bisulfite | HCID 23665763 | — |
| Reactant | HCID 59456262 | HCID 59456262 | — |
| Reactant | Butyllithium | HCID 178418339 | — |
| Solvent | Diethyl Ether | HCID 3283 | — |
| Product | HCID 59456287 | HCID 59456287 | — |
Reaction Steps
24.3 g (about 0.97 mol) of crude 2-propylselenophene are initially introduced in 100 ml of diethyl ether, and 64.5 ml (0.10 mol, 15% soln. in hexane) of n-BuLi are rapidly metered. The mixture is heated under reflux for 1 h and subsequently cooled to −70° C. 16.5 g (0.10 mol) of bromine are added, and the batch is stirred for 1 h at 0° C. and for 3 h at RT. The mixture is added to semi-conc. sodium hydrogensulfite soln., and the organic phase is separated off. The aqueous phase is extracted with MTBE, and the combined organic phases are washed with sat. sodium chloride soln. The solution is dried using sodium sulfate and concentrated to dryness. The residue is purified by vacuum distillation.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08304036B2 |
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| Source dataset | uspto-grants-2012_11 |
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| ORD ID | ord-ce83e9f43406436384e27dff353d4513 |
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| Source note | uspto-grants-2012_11 |
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