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Sodium Hydroxide → N'-(2,6-dichloro-4-trifluoromethylphenyl)-4-cyanobenzohydrazide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | 4-Cyanobenzoyl chloride | HCID 80172 | — |
| 反応物 | [2,6-Dichloro-4-(trifluoromethyl)phenyl]hydrazine | HCID 688223 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | N'-(2,6-dichloro-4-trifluoromethylphenyl)-4-cyanobenzohydrazide | HCID 18471605 | — |
反応手順
A solution of 14.2 g of 4-cyanobenzoyl chloride in 100 ml of methylene chloride is added dropwise with stirring at from 10 to 15° in the course of approximately 30 minutes to 20 g of 2,6-dichloro-4-trifluoromethylphenylhydrazine in 250 ml of dichloromethane, and the mixture is stirred for a further 16 hours. 36 ml of aqueous sodium hydroxide solution (10%) is then run in with vigorous stirring. 100 ml of methylene chloride are added, the organic phase is washed three times using in each case 100 ml of water and dried over sodium sulfate, and the solvent is removed on a rotary evaporator. After the residue has been recrystallized from toluene, the title product of melting point 185-186° is obtained (compound no. 1.6).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06306798B1 |
| 出典データセット | uspto-grants-2001_10 |
| ORD ID | ord-f6a9b79096a94eb8af4cf78b3abf1bad |
| 出典メモ | uspto-grants-2001_10 |