Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Hydrochloric Acid | HCID 313 | — |
| Edukt | Trichloroacetonitrile | HCID 11011 | — |
| Edukt | Bromhydrol | HCID 166749 | — |
| Edukt | Methyl 3-(3-cyanophenyl)prop-2-enoate | HCID 53396017 | — |
| Lösungsmittel | Dichloromethane | HCID 6344 | — |
| Produkt | HCID 57080114 | HCID 57080114 | — |
Reaktionsschritte
Methyl 3-cyanocinnamate (42 pw) is added to a mixture of trichloroacetonitrile (194.4 pw) and aluminum bromide (7.2 pw) in the absence of moisture and at about 25° C. Hydrogen chloride is then introduced over a period of 3 hours with stirring, while keeping the temperature constant. Stirring is discontinued, and the mixture is allowed to react further overnight. In this step, too, a constant temperature of 25° C. is maintained. The solidified mixture is dissolved in 800 pw of dichloromethane, washed with water, and the organic phase is dried over sodium sulfate. Evaporation of the solvent gives a white residue, which is recrystallized from methanol or benzene.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US05064959 |
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| Quelldatensatz | uspto-grants-1991_11 |
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| ORD ID | ord-e7d0a1bdac0446449d77f36e1bb57a4b |
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| Quellennotiz | uspto-grants-1991_11 |
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