| 第 45 卷第 6 期 |  | Vol. 45 No. 6 | | 2015 年 12 月 | Dec 2015 |
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所屬欄目：農藥及中間體
鈀炭催化制備4′-氯-2-氨基聯(lián)苯 |
| 張慧麗，康永利，張 文，王 軒，栗曉東，姚曉龍
（天津市均凱化工科技有限公司，天津 300384） |
| 摘 要：以對氯苯硼酸和鄰氯硝基苯為原料，在N，N-二甲基乙酰胺和水的溶液中以鈀炭為催化劑、碳酸鉀為助催化劑經(jīng)Suzuki反應得4′-氯-2-硝基聯(lián)苯；在乙醇溶液中然后以鋅粉或鐵粉為還原劑回流下還原得到新型殺菌劑啶酰菌胺的關(guān)鍵中間體4′-氯-2-氨基聯(lián)苯�？疾炝蒜Z碳用量、溫度、溶劑配比、堿、反應時(shí)間對反應的影響，優(yōu)化的反應條件為：n（鄰氯硝基苯）∶n（對氯苯硼酸）∶n（鈀碳）∶n（碳酸鉀）=1.00∶1.50∶0.03∶3.00，反應溶劑m（DMAC）∶m（水）=30∶1；反應溫度為130℃，碳酸鉀為弱堿，反應時(shí)間為12 h。優(yōu)化條件下反應收率69.43%，該路線(xiàn)具有原材料易得、成本低、催化劑可回收套用等優(yōu)點(diǎn)。 |
| 關(guān)鍵詞：啶酰菌胺；4′-氯-2-氨基聯(lián)苯；對氯苯硼酸；鄰氯硝基苯 |
| 中圖分類(lèi)號：TQ2 文獻標識碼：A 文章編號：1009-9212（2015）05-0010-04 |
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| Preparation of 4′-Chloro-2-aminobiphenyl Using Palladium Carbon as Catalyst |
| ZHANG Hui-li, KANG Yong-li, ZHANG Wen, WANG Xuan, LI Xiao-dong, YAO Xiao-long
(Tianjin Junkai Chemical Co., Ltd., Tianjin 300384,China) |
| Abstract：Using 4-chlorophenylboronic acid and 2-nitrochlorobenzene as raw materials, palladium carbon and alkali as catalyst in N,N-dimethylacetamide and water, the reaction mixture was heated to 130℃ for 12 hours by Suzuki reaction to give 4′-chloro-2-nitro-biphenyl. Then, 4′-chloro-2-nitro-biphenyl was reduced by zinc powder or iron powder in ethanol at reflux to give 4′-chloro-2-aminobipheny, a key intermediate of the new fungicide Boscalid. The amount of palladium carbon, temperature of the reaction, the ratio of solvent, alkali and reaction time was evaluated. The optimum reaction conditions were as following: n(2-nitrochlorobenzene):n(4-chlorophenylboronic acid):n(palladium carbon):n(potassium carbonate)=1.00:1.50:0.03:3.00; the weight ratio of DMAC to water was 30:1; reaction temperature was 130℃; potassium carbonate was used as the alkali; the reaction time was 12 h. The route had advantages of low cost, no phosphours ligands, easy to obtain raw materials, the catalyst recycling, environment friendly, etc. |
| Key words：boscalid; 4′-chloro-2-aminobiphenyl; 4-chlorophenylboronic acid; 2-nitrochlorobenzene |
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基金項目：天津市科技支撐計劃重點(diǎn)項目（15ZCZDNC00100）。
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作者簡(jiǎn)介：張慧麗（1983-），女，河北石家莊人，碩士，研究方向：農藥醫藥中間體合成。
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收稿日期： 2015-09-1
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