化工社化工社 化学情報印刷レポート · 研究参考用
Carbon Dioxide → 3-Cyano-2,4-dichlorobenzoic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Carbon Dioxide | HCID 280 | — |
| 反応物 | Water | HCID 962 | — |
| 反応物 | Dichlobenil | HCID 3031 | — |
| 反応物 | Lithium diisopropylamide | HCID 2724682 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 3-Cyano-2,4-dichlorobenzoic acid | HCID 54073181 | — |
反応手順
A solution of lithium di-isopropylamide (2M in heptane, 25 ml) was added to a solution of 2,6-dichlorobenzonitrile (8.6 g) in THF while maintaining the temperature below -70° C. The mixture was stirred for 1.5 hours then poured onto solid carbon dioxide. It was stirred for 1 hour then diluted with ether. Water was added and the mixture was acidified to pH1. It was extracted with ether, washed with water, dried (MgSO4) and filtered. The filtrate was evaporated to dryness to give 3-cyano-2,4-dichlorobenzoic acid (9.4 g) as a white solid mp 230°-232° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05859283 |
| 出典データセット | uspto-grants-1999_01 |
| ORD ID | ord-c92932fa4ed3427f805ed3fe020bc414 |
| 出典メモ | uspto-grants-1999_01 |