Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Methanesulfonic Acid | HCID 6395 | — |
| Reactant | HCID 67451391 | HCID 67451391 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | HCID 67451857 | HCID 67451857 | — |
Reaction Steps
16.4 g (43.6 mmol) of 2-(5-bromo-2-carbazol-9-ylphenyl)propan-2-ol are dissolved in 1200 ml of degassed toluene, a suspension of 40 g of polyphosphoric acid and 28 ml of methanesulfonic acid is added, and the mixture is heated at 60° C. for 1 h. The batch is cooled, and water is added. A solid precipitates out and is dissolved in methylene chloride/THF (1:1). The solution is carefully rendered alkaline using 20% NaOH, the phases are separated and dried over MgSO4. The solid obtained is washed by stirring with heptane. Yield: 14.8 g (40 mmol), 95% of theory, purity according to 1H-NMR about 95%.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US09422287B2 |
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| Source dataset | uspto-grants-2016_08 |
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| ORD ID | ord-6e81af197d21458aad39886f31599b29 |
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| Source note | uspto-grants-2016_08 |
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