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1,1-Dichloroethane → 2,4-Dichlorobenzonitrile
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 1,1-Dichloroethane | HCID 6365 | — |
| 反応物 | 4-Chloro-2-nitrobenzonitrile | HCID 96924 | — |
| 反応物 | Lithium Chloride | HCID 433294 | — |
| 反応物 | Aluminum(III) Chloride | HCID 6451240 | — |
| 溶媒 | N-methyl-2-pyrrolidone | HCID 13387 | — |
| 生成物 | 2,4-Dichlorobenzonitrile | HCID 81050 | 79.2% |
反応手順
4.55 parts of 4-chloro-2-nitrobenzonitrile, 0.42 parts of lithium chloride, 1.11 parts of anhydrous aluminum chloride and 15 parts of N-methyl-2-pyrrolidone were reacted at 180° C. for 3 hours after the pattern of EXAMPLE B1. The reaction solution was added with 100 parts of dichloroethane, agitated for 30 minutes and filtered. Dichloroethane was distilled off from the filtrate and the residue was added with water to precipitate the crude crystals. The crude crystals were recrystallized by using a water-methanol mixed solvent to obtain 3.4 parts of 2,4-dichlorobenzonitrile with purity of 99%. Yield: 79.2%.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04225534 |
| 出典データセット | uspto-grants-1980_09 |
| ORD ID | ord-402a1150f9fe498699052d6d9e667ac6 |
| 出典メモ | uspto-grants-1980_09 |