| 第 45 卷第 1 期 |  | Vol. 45 No. 1 | | 2015 年 2 月 | Feb 2015 |
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所屬欄目：農藥及中間體
2-氰基-2，2-二（4-氯芐基）乙酸乙酯的合成研究 |
| 田宗明，秦永華，張 斌，金小平
（浙江醫藥高等專(zhuān)科學(xué)校 生物與制藥學(xué)院，浙江 寧波 315100） |
| 摘 要：以4-氯甲苯為原料，二氯甲烷為溶劑，室溫下，用三氯化硼氯化甲基側鏈合成4-氯氯芐，收率55.3%；乙醇鈉催化下，物料配比 n（4-氯氯芐）∶n（丙二腈）=2.0∶1.0，反應合成2，2-二（4-氯芐基）丙二腈，收率51.2%；有水的條件下，二氯亞砜催化，乙醇醇解2，2-二（4-氯芐基）丙二腈合成2-氰基-2，2-二（4-氯芐基）乙酸乙酯，收率62.9%。產(chǎn)物結構經(jīng)IR、1H NMR及X單晶結構衍射確證。 |
| 關(guān)鍵詞：乙酸乙酯；4-氯芐基；丙二腈 |
| 中圖分類(lèi)號：O622.2 文獻標識碼：A 文章編號：1009-9212（2015）01-0019-05 |
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| Synthesis of 2-Cyano-2, 2-bis(4-fluorobenzyl)ethyl Acetate |
| TIAN Zong-ming, QIN Yong-hua, ZHANG Bin, JIN Xiao-ping
(Zhejiang Pharmaceutical College, Ningbo 315100, China) |
| Abstract：A yield of 55.3% for the preparation of 4-chloromethylbenzyl chloride was achieved using 4-chloro-toluene as the raw material, boron trichloride as the chlorination agent at room temperature. Then, 4-Chlorobenzyl chloride was reacted with malononitrile to give 2,2-bis(4-chlorobenzyl)malononitrile, and a yield of 51.2% was obtained at 4-Chloro benzyl chloride/malononitrile ratio of 2.0:1.0 using sodium ethoxide as catalyst. At the presence of water and thionyl chloride as the catalyst, a yield of 62.9% for 2-cyano-2,2-bis(4-chloridebenzyl)ethyl acetate was achieved using ethanol alcoholization reaction of 2,2-bis(4-chlorobenzyl)malononitrile, and the molecular structure of this product was characterized using IR, 1H NMR and X-ray diffraction. |
| Key words：ethyl acetate; 4-fluorobenzyl; malononitrile |
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基金項目：浙江省自然科學(xué)基金（LQ13B010004），浙江醫藥高等專(zhuān)科學(xué)�？蒲许椖浚╖PCSR2011006）。
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作者簡(jiǎn)介：田宗明（1978-），男，湖北宣恩人，講師，碩士，研究方向：藥物及中間體合成（E-mail：tzmming@163.com）。
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收稿日期： 2014-11-1
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