関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Aluminum(III) Chloride | HCID 6451240 | — |
| 反応物 | 2-(5-Bromo-6-methoxy-2-naphthyl)propionitrile | HCID 14073055 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 溶媒 | Mesitylene | HCID 7947 | — |
| 生成物 | 2-(6-Methoxynaphthalen-2-yl)propanenitrile | HCID 607344 | 71% |
反応手順
10 Grams of anhydrous aluminum chloride are added portionwise and under stirring to a solution containing 14.5 g of 2-(5-bromo-6-methoxy-2-naphthyl)propionitrile dissolved in 60 ml of methylene chloride and 8.3 ml of mesitylene, while keeping the temperature at about 20° C. The reaction mixture is kept at this temperature under stirring for 1 hour and then is slowly poured into a mixture made of 60 g of crushed ice and of 20 ml of a 6N aqueous solution of hydrochloric acid. The layers are separated after 15 minutes of stirring and the aqueous layer is discarded. The organic layer is twice washed with 25 ml of a 6N aqueous solution of hydrochloric acid, then with 25 ml of water and is dried over anhydrous sodium sulfate. The organic solution is evaporated to dryness under vacuum and the residue is crystallized from tetrachloroethylene obtaining 7.5 g of product with a yield of 71%.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US05107013 |
|---|
| 出典データセット | uspto-grants-1992_04 |
|---|
| ORD ID | ord-ae40c9524c794c9f9020bfc134b647e7 |
|---|
| 出典メモ | uspto-grants-1992_04 |
|---|