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Potassium Iodide → N,N-dimethyl N'-[2-(3-pyridyl)ethyl]ethanediamine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Potassium Iodide | HCID 4875 | — |
| 反応物 | Pyridine, 3-(2-chloroethyl)-, hydrochloride | HCID 199465 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | N~1~,N~1~-Dimethylethane-1,1-diamine | HCID 18943179 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | N,N-dimethyl N'-[2-(3-pyridyl)ethyl]ethanediamine | HCID 18788472 | 56.1% |
反応手順
11 g of 3-(2-chloroethyl)pyridine hydrochloride, 16.3 g of N,N-dimethylethane diamine, 18.5 g of sodium bicarbonate and 13 g of potassium iodide are heated in 150 ml of ethanol for about 30 hours at about 60° C. The solvent is evaporated and the residue is taken up in 100 ml of water before an aqueous solution of 10N NaOH is added to give pH 8; the aqueous phase is then extracted 3 times with 80 ml of ethyl acetate. The pooled organic phases are dried over magnesium sulfate, filtered and concentrated under reduced pressure. The residual oil is distilled to give 6.7 g of the expected product. B.p.=100-107° C./10 Pa.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05891894 |
| 出典データセット | uspto-grants-1999_04 |
| ORD ID | ord-4c750b6964504f4f94050395f50a6321 |
| 出典メモ | uspto-grants-1999_04 |