Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Sulfuric Acid | HCID 1118 | — |
| Reactant | HCID 15032031 | HCID 15032031 | — |
| Solvent | Nitrobenzene | HCID 7416 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 15032032 | HCID 15032032 | 102.1% |
Reaction Steps
To a 50 ml 3-neck round bottom flask is charged 2 g product of Example 2 in 10 ml nitrobenzene. 0.1 ml H2SO4 is added and isobutylene is bubbled through the solution while warming to 90° C. After TLC shows the reaction to be complete, the mixture is diluted with an equal volume of ethyl acetate and washed 2 times with 50 ml 5% sodium bicarbonate. The organic layer is dried and concentrated in vacuo. The residue is purified by dry column chromatography (Et2O/hexane) to yield 1.3 g of product, mp 215°-217° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US04826983 |
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| Source dataset | uspto-grants-1989_05 |
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| ORD ID | ord-d3b211d1d53c46a8b6a409bada275ac3 |
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| Source note | uspto-grants-1989_05 |
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