関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 4-Nitroaniline | HCID 7475 | — |
| 反応物 | 2-Diazonio-1-methoxy-3-oxobut-1-en-1-olate | HCID 54537960 | — |
| 触媒 | Dirhodium tetraacetate | HCID 152122 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | Methyl 2-[(4-nitrophenyl)amino]-3-oxobutanoate | HCID 70968068 | 98% |
反応手順
Under an argon atmosphere, to a solution of 4-nitroaniline (3.84 g) in toluene (278 mL) were added methyl 2-diazo-3-oxobutanoate (5.13 g) and rhodium(II) acetate dimer (250 mg), and the mixture was stirred at 120° C. for 1 hr. The solvent was evaporated under reduced pressure, and the residue was purified by silica gel column chromatography [eluent; hexane:ethyl acetate=9:1→hexane:ethyl acetate=7:3 (volume ratio)] to give the title compound (4.63 g, yield 98%) as a yellow solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08642770B2 |
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| 出典データセット | uspto-grants-2014_02 |
|---|
| ORD ID | ord-1cfa878266b04a4fb7715964e4164ab7 |
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| 出典メモ | uspto-grants-2014_02 |
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