関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Acrylic Acid | HCID 6581 | — |
| 反応物 | 1-Bromo-4-iodo-2-methoxybenzene | HCID 12187202 | — |
| 触媒 | palladium(II) acetate | HCID 167845 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | 4-Bromo-3-methoxycinnamic acid | HCID 58005127 | — |
反応手順
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.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08314062B2 |
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| 出典データセット | uspto-grants-2012_11 |
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| ORD ID | ord-30ec2bea95874b05a1ce95d501715363 |
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| 出典メモ | uspto-grants-2012_11 |
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