Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Chloride | HCID 312 | — |
| Reactant | t-Butyl bromide | HCID 10485 | — |
| Reactant | Potassium Hydroxide | HCID 14797 | — |
| Reactant | HCID 86757894 | HCID 86757894 | — |
| Solvent | Ethanol | HCID 702 | — |
| Solvent | Diethyl Ether | HCID 3283 | — |
| Product | HCID 86757893 | HCID 86757893 | — |
Reaction Steps
6.2 g (0.11 mol) of potassium hydroxide was dissolved in 250 ml of ethanol. 27.2 g (0.05 mol) of bis-(4-hydroxyphenyliodonium) 3,3,3,2,1,1-hexafluoropropane sulfonate (prepared from a metathesis reaction of chloride) was added to the solution. The mixture was stirred for 3 hours. The solution was then heated to 50° C., and 15.1 g (0.11 mol) of t-butyl bromide was added dropwise thereto. The mixture was heated under reflux for 6 hours. The precipitates were removed by filtration. The solvent was removed from the filtrate by distillation. The residue was dissolved in 250 ml of ethyl acetate. The solution was washed several times with water, and then dried. The solvent was removed to obtain a yellow oil. The contemplated material was obtained by recrystallization from diethyl ether. The structure was confirmed by 1H-NMR (CDCl3): δ=1.43 (s, 18H), 5.00-5.30 (d[m], 1H), 7.17-7.21 (d, 4H), 7.55-7.59 ppm (d, 4H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06358665B1 |
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| Source dataset | uspto-grants-2002_03 |
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| ORD ID | ord-a27af7f619e54ed493fa0f2284618393 |
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| Source note | uspto-grants-2002_03 |
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