関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ethyl isobutyrate | HCID 7342 | — |
| 反応物 | Tetrahydrofuran | HCID 8028 | — |
| 反応物 | 2-Bromo-6-methoxypyridine | HCID 256810 | — |
| 反応物 | Lithium Hexamethyldisilazide | HCID 2733832 | — |
| 触媒 | Tris(1,1-dimethylethyl)phosphine | HCID 83681 | — |
| 触媒 | Bis(dibenzylideneacetone)palladium | HCID 9811564 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 2-(6-Methoxy-pyridin-2-yl)-2-methyl-propionic acid ethyl ester | HCID 66834925 | 64.4% |
反応手順
2-Bromo-6-methoxypyridine (7.0 g), ethyl isobutyrate (4.75 g), tri t-butylphosphine (300 mg) and Pd2(dba)3 (680 mg) were dissolved in toluene (200 ml) under nitrogen atmosphere, added with THF solution of LiHMDS (1.6 M, 24 ml), and the mixture was stirred at 100° C. for 6 hrs. The reaction mixture was diluted with ethyl acetate (300 ml), and washed three times with 15% brine (200 ml). The organic layer was concentrated under reduced pressure and the resulting residues were purified by silica gel column (n-hexane/ethyl acetate=4/1) to obtain the title compound (5.353 g, yield 60%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US09440922B2 |
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| 出典データセット | uspto-grants-2016_09 |
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| ORD ID | ord-e6f1d85672d846248de4662bd3f783e2 |
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| 出典メモ | uspto-grants-2016_09 |
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