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Acetic Anhydride → 2-Chloro-3-(2-nitroethenyl)pyridine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Acetic Anhydride | HCID 7918 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Ethylamine hydrochloride | HCID 11198 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | 2-Chloro-3-pyridinecarboxaldehyde | HCID 737607 | — |
| 触媒 | 4-(Dimethylamino)pyridine | HCID 14284 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 溶媒 | Nitromethane | HCID 6375 | — |
| 生成物 | 2-Chloro-3-(2-nitroethenyl)pyridine | HCID 86647802 | — |
反応手順
To 2-chloronicotinaldehyde (2.8 g, 19.8 mmol) in nitromethane (6.1 g) was added ethylamine hydrochloride (100 mg, 1.2 mmol) and NaOH (25 mg) in ethanol (1.5 mL). The mixture was stirred for 1 hour and concentrated. The crude was dissolved in CH2Cl2 (30 mL) and treated with triethylamine (2.8 g, 28 mmol), 4-(dimethylamino)pyridine (20 mg) and acetic anhydride (2.0 g, 20 mmol) at 0° C. The mixture was stirred for 15 minutes and concentrated saturated NaHCO3(aq) was added, and the precipitates were collected to afford the title compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09187483B2 |
| 出典データセット | uspto-grants-2015_11 |
| ORD ID | ord-04009455b9f14af6a61938db44567b12 |
| 出典メモ | uspto-grants-2015_11 |