関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | Benzeneacetonitrile, 4-fluoro- | HCID 68016 | — |
| 反応物 | p-(Hexyloxy)benzaldehyde | HCID 79816 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | HCID 19885222 | HCID 19885222 | 20% |
反応手順
A solution of 51.5 g of 4-hexyloxybenzaldehyde and 33.8 g of 4-fluorophenylacetonitrile in methanol was stirred at room temperature and aqueous sodium hydroxide (50 percent) was added dropwise until a precipitate appeared. Water was then added and the solids were collected by filtration to render α-[[4-(hexyloxy)phenyl]methylene]-4-fluorophenylacetonitrile which was reduced as follows. 40.2 g of said nitrile, 10 g of Raney nickel, 150 ml of anhydrous ammonia and 300 ml of tetrahydrofuran were stirred at 110° for 12 hours at a pressure of 2000 psi. The catalyst and solvent were removed and the hydrochloride salt was made in the filtrate by the addition of anhydrous hydrochloric acid. Recrystallization from methanol rendered the title compound (20 percent yield).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US05135955 |
|---|
| 出典データセット | uspto-grants-1992_08 |
|---|
| ORD ID | ord-90628494bc12430485abf93a5704b848 |
|---|
| 出典メモ | uspto-grants-1992_08 |
|---|