Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Butanedione | HCID 650 | — |
| Edukt | HCID 178418255 | HCID 178418255 | — |
| Lösungsmittel | Tetrahydrofuran toluene | HCID 22635083 | — |
| Produkt | 3-Hydroxy-3-phenylbutan-2-one | HCID 233220 | 66,4% |
Reaktionsschritte
The process can also be run in mixtures of tetrahydrofuran and toluene, thereby making the process more economical. When 1.1 equivalent of phenylmagnesium bromide (1.9M in 50% THF/PhMe) was added to 2,3-butanedione in 50% THF/PhMe, crude product was isolated in 82.4% yield (Run 10, Table IV) after work-up. Short path vacuum distillation gave 3-hydroxy-3-phenylbutan-2-one in 68% yield. Alternatively, preparation of phenylmagnesium bromide in 38% THF/PhMe, followed by reaction with 2,3-butanedione in 38% THF/PhMe afforded 3-hydroxy-3-phenylbutan-2-one in 66.4% yield (Run 11, Table IV) after work-up and distillation. Similarly phenylmagnessium bromide in 25% THR/PheMe reacted with 2,3-butanedione in 25% THF/PheMe yielded 3-hydroxy-3-phenylbutan-2-one in 56.9% yield after work-up and distillation.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US04704475 |
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| Quelldatensatz | uspto-grants-1987_11 |
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| ORD ID | ord-df0cec7d1a924982811e613865350924 |
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| Quellennotiz | uspto-grants-1987_11 |
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