関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Benzonitrile, 4-bromo- | HCID 12162 | — |
| 反応物 | Binap, (A+-)- | HCID 634876 | — |
| 反応物 | Sodium bis(trimethylsilyl)amide | HCID 2724254 | — |
| 反応物 | HCID 178435110 | HCID 178435110 | — |
| 触媒 | Bis(dibenzylideneacetone)palladium | HCID 9811564 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | HCID 178461988 | HCID 178461988 | — |
反応手順
To a mixture of 2-((S)-1-(2-fluorophenyl)ethylamino)-5-methylthiazol-4(5H)-one (0.0500 g, 0.198 mmol), 4-bromobenzonitrile (Aldrich, 0.0721 g, 0.396 mmol), Pd2(dba)3 (Aldrich, 0.0127 g, 0.0139 mmol), 2-(diphenylphosphino)-1-(2-(diphenylphosphino)naphthalen-1-yl)naphthalene (Strem, 0.0123 g, 0.0198 mmol), and NaN(TMS)2 (Aldrich, 0.0727 g, 0.396 mmol) was added toluene (2 mL) in a dry box. The mixture was gradually heated to 95° C. and stirred overnight. The reaction was cooled to ambient temp. and quenched with NH4Cl (5 mL). The reaction mixture was extract with EtOAc. The organic phase was dried over Na2SO4, filtered, and concentrated in vacuo. The crude product was purified by silica gel chromatography. MS: 354 (M+1)
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08541592B2 |
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| 出典データセット | uspto-grants-2013_09 |
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| ORD ID | ord-186e9403d5944feca041a124aeb48779 |
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| 出典メモ | uspto-grants-2013_09 |
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