Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Acetone | HCID 180 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | 2-Butene, 1-bromo-3-methyl- | HCID 70092 | — |
| Reactant | 2-Cyano-6-hydroxybenzothiazole | HCID 9881912 | — |
| Solvent | Ethylacetate heptane | HCID 21899848 | — |
| Product | HCID 66702726 | HCID 66702726 | 124.3% |
Reaction Steps
To a dry 25-ml round-bottomed flask containing acetone (5 mL), anhydrous potassium carbonate (1.2 g, 8.4 mmol), and prenyl bromide (839 microliters, 7.3 mmole) was added 6-hydroxy-2-cyanobenzothiazole (1.0 g, 5.6 mmol). The mixture was refluxed under argon with stirring. Reaction progress was monitored by TLC analysis, developing with 2:1 heptane-ethyl acetate. After 28 h, the potassium carbonate was filtered from the cooled reaction mixture. The solution was concentrated in vacuo to yield 1.7 g of solid. The solid was further purified by flash chromatography using 9:1 heptane-ethyl acetate and gradually stepping to 4:1 heptane-ethyl acetate. Appropriate fractions were pooled and evaporated to yield 0.8 g of solid. The structure was confirmed by 1H NMR analysis in DMSO-d6.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08765969B2 |
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| Source dataset | uspto-grants-2014_07 |
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| ORD ID | ord-f5b2346b0f084417a3283b897f18aad3 |
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| Source note | uspto-grants-2014_07 |
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