化工社化工社 化学情報印刷レポート · 研究参考用
1,2-Dichloroethane → 3-(Acetoxymethyl)benzonitrile
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 1,2-Dichloroethane | HCID 11 | — |
| 反応物 | Water | HCID 962 | — |
| 反応物 | Benzonitrile, 3-(aminomethyl)- | HCID 457594 | — |
| 反応物 | Sodium Nitrite | HCID 23668193 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 生成物 | 3-(Acetoxymethyl)benzonitrile | HCID 10012422 | 78% |
反応手順
m-Cyanobenzylamine (13.2 g), water (18 g), and 1,2-dichloroethane (22 g) were mixed, and the mixture was stirred with cooling with ice. Acetic acid (18 g) was added to the mixture. Subsequently, a 20 wt % aqueous solution (51.8 g) of sodium nitrite was added dropwise to the mixture over a one hour period. The mixture was stirred at the same temperature for four hours. The reaction mixture was subjected to extraction with 1,2-dichloroethane, and the organic solvent was concentrated. Water was added to the concentrated solution, and the residual organic solvent was removed through distillation, to thereby obtain 13.7 g of m-cyanobenzyl acetate (yield 78%). The purity of the product was 97%.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06187945B1 |
| 出典データセット | uspto-grants-2001_02 |
| ORD ID | ord-fe93df3edc0e4ce399cb5aa40e46f37a |
| 出典メモ | uspto-grants-2001_02 |