関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Sodium Iodide | HCID 5238 | — |
| 反応物 | Ammonium Hydroxide | HCID 14923 | — |
| 反応物 | 1-(3,5-Dimethylphenoxy)-2-chloropropane | HCID 19100307 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 生成物 | 2-(3,5-Dimethyl-phenoxy)-1-methyl-ethylamine | HCID 5305257 | 83.7% |
反応手順
A 100 ml autoclave was charged with 1.96 g (9.8 mmol) of 1-(3,5-dimethylphenoxy)-2-chloropropane, 10 ml of ethanol and 0.2 g of sodium iodide, and then 40 ml of a 28% ammonia aqueous solution was added. The mixture was continuously stirred at 130° C. for 8 hours to complete the reaction. After allowed to cool, the reaction mixture was transferred into a 500 ml beaker with 50 ml of water and 20 ml of diethyl ether. A 20% hydrochloric acid aqueous solution was added to the reaction mixture until it became acidic, and the mixture was washed with 20 ml of diethyl ether three times. While the water layer was cooled, a 20% sodium hydroxide aqueous solution was added to make it alkaline, and the water layer was subjected to extraction with 50 ml of diethyl ether three times, and dried over 10 g of anhydrous sodium sulfate. Then, the solvent was distilled off under reduced pressure to give 1.48 g of 1-(3,5-dimethylphenoxy)-2-aminopropane (yield 83.7%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US05286905 |
|---|
| 出典データセット | uspto-grants-1994_02 |
|---|
| ORD ID | ord-36a4dc3bc9f2489da306b91df0987b8e |
|---|
| 出典メモ | uspto-grants-1994_02 |
|---|