Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Hydrochloric Acid | HCID 313 | — |
| Edukt | Acrylic Acid | HCID 6581 | — |
| Edukt | 1-Bromo-4-iodo-2-methoxybenzene | HCID 12187202 | — |
| Katalysator | palladium(II) acetate | HCID 167845 | — |
| Lösungsmittel | Acetonitrile | HCID 6342 | — |
| Produkt | 4-Bromo-3-methoxycinnamic acid | HCID 58005127 | — |
Reaktionsschritte
To a solution of 1-bromo-4-iodo-2-methoxybenzene (L. A. Hasvold et al., US 2004/0254159) in MeCN (1.1 M) was added acrylic acid (1.24 eq.), TEA (2.5 eq.) and palladium acetate (0.03 eq). The reaction mixture was heated to 90° C. for 40 min, cooled to RT and poured into 1N HCl. After sting for 30 min, the solid was filtered, heated to reflux in EtOH (2.3 M), allowed to cool to RT and stirred overnight. The solid was filtered and washed with 1:1 EtOH:hexane to give the desired product 119. LRMS ESI+ (M+H)+ 257.0.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US08314062B2 |
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| Quelldatensatz | uspto-grants-2012_11 |
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| ORD ID | ord-30ec2bea95874b05a1ce95d501715363 |
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| Quellennotiz | uspto-grants-2012_11 |
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