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Sodium Carbonate → 3-Chloro-2-(2,4-dichlorophenylthio)-nitrobenzene
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium Carbonate | HCID 10340 | — |
| 反応物 | 2,3-Dichloronitrobenzene | HCID 18555 | — |
| 反応物 | 2,4-Dichlorobenzenethiol | HCID 70730 | — |
| 溶媒 | O-Xylene | HCID 7237 | — |
| 生成物 | 3-Chloro-2-(2,4-dichlorophenylthio)-nitrobenzene | HCID 21697868 | — |
反応手順
Sodium carbonate (13.8 g) is added to a solution of 1,2-dichloro-3-nitrobenzene (19.29 g) and 2,4-dichlorothio-phenol (17.9 g) in xylene (250 ml), and the resulting mixture is heated for 5 hours at reflux temperature. The precipitate is separated by filtration, washed with xylene and the combined organic phases are concentrated. The resultant residue is mixed with petroleum ether and stirred for 1 hour at room temperature. Following this, the crystalline material is suction filtered and washed with petroleum ether, and any remaining solvent is removed in a vacuum. Yield: 25.6 g of colourless crystals (76.6%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06297282B1 |
| 出典データセット | uspto-grants-2001_10 |
| ORD ID | ord-2fb5417e2cc842c6ac1694a12d2490dc |
| 出典メモ | uspto-grants-2001_10 |