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Triethylamine → 4-(3-Nicotinoylaminopropyloxy)pyridine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 3-Pyridinecarbonyl chloride, hydrochloride (1:1) | HCID 88438 | — |
| 反応物 | 4-(3-Aminopropoxy)pyridine | HCID 14994125 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 4-(3-Nicotinoylaminopropyloxy)pyridine | HCID 19079167 | 88.7% |
反応手順
To a solution of 700 mg (4.60 mmol) of 4-(3-aminopropyloxy)pyridine and 1.54 ml (11.0 mmol) of triethylamine in 30 ml of methylene chloride, 830 mg (4.66 mmol) of nicotinoyl chloride hydrochloride was added under ice-cooling with stirring. The mixture was stirred at room temperature for 1.5 hours. The reaction mixture was washed successively with a saturated aqueous solution of sodium bicarbonate and brine and dried over anhydrous magnesium sulfate, and then the solvent was distilled off. The residue was purified by column chromatography (eluent: ethanol/ethyl acetate=1:10 to 1:5) to obtain 1.05 g of the desired compound (yield: 85.8%, colorless crystals).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05246948 |
| 出典データセット | uspto-grants-1993_09 |
| ORD ID | ord-21c6230f734548bda488fe39bf56a85a |
| 出典メモ | uspto-grants-1993_09 |