関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | tert-Butyl acrylate | HCID 15458 | — |
| 反応物 | 2-Amino-5-bromopyridine | HCID 70622 | — |
| 反応物 | Tri-o-tolylphosphine | HCID 80271 | — |
| 触媒 | palladium(II) acetate | HCID 167845 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | 3-(6-Amino-pyridin-3-yl)-acrylic acid tert-butyl ester | HCID 53665462 | — |
反応手順
A mixture of 2-amino-5-bromopyridine 10-1 (10 g, 58 mmol), tert-butyl acrylate (50 mL, 344 mmol), triethylamine (50 mL, 359 mmol), tri-o-tolylphosphine (3.0 g, 9.8 mmol) and Pd(OAc)2 (1.0 g, 4.5 mmol) in 150 mL CH3CN was purged with argon for 5 min and subsequently refluxed at 110° C. for 20 hr. The mixture was then cooled and concentrated. The residue was purified using silica gel flash chromatography (EtOAc/hexanes 1:1) to afford the desired product 10-2 as a solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US06066648 |
|---|
| 出典データセット | uspto-grants-2000_05 |
|---|
| ORD ID | ord-7f4efd1108bb45e5aa2b0660aa26cc90 |
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| 出典メモ | uspto-grants-2000_05 |
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