関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Acetic Acid | HCID 176 | — |
| 反応物 | 2-Methyl-2-nitropropane | HCID 11672 | — |
| 反応物 | 2,4-Difluorobenzaldehyde | HCID 73770 | — |
| 触媒 | Zinc | HCID 23994 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | alpha-(2,4-difluorophenyl)-N-t-butylnitrone | HCID 73770286 | — |
反応手順
To a suspension of 2,4-difluorobenzaldehyde (608.9 mg, 4.28 mmol), 1,1-dimethylnitroethane (881.9 mg, 8.55 mmol) and zinc (840.0 mg, 12.8 mmol) in ethanol (15 ml) was added acetic acid (1.54 g, 25.6 mmol) dropwise at 5° C. while stirring. The mixture was stirred at room temperature for one day. After the mixture was cooled to 5° C., zinc acetate was filtered off and the filtrate was concentrated and purified by silica gel chromatography (hexane/ethyl acetate=4/1).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US06194461B1 |
|---|
| 出典データセット | uspto-grants-2001_02 |
|---|
| ORD ID | ord-13e2320fe3994b55bbfbcaa192369478 |
|---|
| 出典メモ | uspto-grants-2001_02 |
|---|
