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Benzonitrile → 3-Amino-5-(tert-butyl)-2-methoxybenzonitrile
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Benzonitrile | HCID 7505 | — |
| 反応物 | Ammonium formate | HCID 2723923 | — |
| 触媒 | Palladium | HCID 23938 | — |
| 溶媒 | Ethylacetate methanol | HCID 21584119 | — |
| 生成物 | 3-Amino-5-(tert-butyl)-2-methoxybenzonitrile | HCID 21097297 | 153.6% |
反応手順
The above benzonitrile (100 mg, 0.427 mmol) was dissolved in 1:1 ethyl acetate/methanol (10 mL) in a nitrogen-flushed flask. Ammonium formate (270 mg, 4.27 mmol) and palladium on carbon (30 mg, 10% wet) were added and the mixture was heated to reflux for 30 min. The reaction was cooled to room temperature and filtered through a pad of diatomaceous earth, eluting with ethyl acetate. The ethyl acetate was evaporated under vacuum. The resulting residue was purified by chromatography on silica gel (1:1 ethyl acetate/hexanes) to afford the title compound, (67 mg, 77%) as a colorless oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07285545B2 |
| 出典データセット | uspto-grants-2007_10 |
| ORD ID | ord-6dbeb552a2974150b0097febf485c68d |
| 出典メモ | uspto-grants-2007_10 |