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2-Dimethylaminopyridine → Ethyl 5-(acetylamino)-2-bromobenzoate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 2-Dimethylaminopyridine | HCID 21885 | — |
| 反応物 | 1-Hydroxybenzotriazole | HCID 75771 | — |
| 反応物 | 5-Acetamido-2-bromobenzoic acid | HCID 2734159 | — |
| 反応物 | 1-(3-Dimethylaminopropyl)ethylcarbodiimide hydrochloride | HCID 21982921 | — |
| 溶媒 | Dichloromethane ethanol | HCID 21584144 | — |
| 生成物 | Ethyl 5-(acetylamino)-2-bromobenzoate | HCID 69309519 | 76.2% |
反応手順
A mixture of 5-(acetylamino)-2-bromobenzoic acid (2.58 g, 10 mmol), 1-hydroxybenzotriazole (1.68 g, 11 mmol), dimethylaminopyridine (1.22 g, 10 mmol) and 1-(3-dimethylaminopropyl)-ethylcarbodiimide hydrochloride (2.20 g, 11.5 mmol) in dichloromethane/ethanol (5:1, 30 ml) was stirred at room temperature for 2 hours then washed with saturated sodium bicarbonate solution, dried (magnesium sulphate) and chromatographed on silica eluting with ethyl acetate/iso-hexane (2:3) to give 2.18 g of white solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07446222B2 |
| 出典データセット | uspto-grants-2008_11 |
| ORD ID | ord-943100f8158e4b6f8c445f41bf2972e8 |
| 出典メモ | uspto-grants-2008_11 |