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2-(1-H-四唑)-4'-甲基联苯的合成 被引量：1

Synthesis of 5-(4'-Methyl-[1,1'-biphenyl]-2-yl)-1H-tetrazole
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摘要 以2-氰基-4'-甲基联苯(Ⅱ)为原料,与氨基钠反应得到2-脒基-4'-甲基联苯(Ⅲ),该化合物与水合肼发生取代反应得到4'-甲基-[1,1'-联苯]-2-甲酰胺酰肼(Ⅳ),最后在酸性条件下与亚硝酸钠发生闭环反应得到2-(1-H-四唑)-4'-甲基联苯(Ⅰ),总收率达到81%,其结构经1HNMR和MS确证。 5- （ 4＇-Methyl- [ 1,1 ＇-biphenyl ] -2-yl ） -1H-tetrazole was synthesized from 4＇-methyl- [ 1,1 ＇- biphenyl ]-2-carbonitrile as the starting material in a total yield of 81%. 4＇-Methyl-[ 1,1 ＇-biphenyl ]-2- carboximidamide （ m ） was firstly obtained by the addition of 4＇-methyl-[ 1,1 ＇-biphenyl ]-2-carbonitrile with sodium amide in toluene. The subsequent substitution reaction of m with hydrazine hydrate resulted in the formation of 4＇-methyl- [ 1,1 ＇-biphenyl ] -2-earboximidhydrazide （ IV ）, and the final acidic cyclization of IV with sodium nitrite gave the title compound 5- （ 4＇-methyl- [ 1,1 ＇-biphenyl ] -2- yl）-lH-tetrazole（ I ）,whose structure was characterized by means of 1HNMR and MS.
作者 汪家宏 沈叶楠 龙中柱 张程亮 王巧纯
机构地区 华东理工大学精细化工研究所结构可控先进功能材料及其制备教育部重点实验室 启东东岳药业有限公司
出处 《精细化工》 EI CAS CSCD 北大核心 2015年第5期598-600,共3页 Fine Chemicals
基金 江苏省企业院士工作站(BM2013038)~~
关键词 2-(1-H-四唑)-4'-甲基联苯 沙坦联苯 四氮唑 精细化工中间体 5 - （ 4 ＇-methyl- [ 1,1 ＇-biphenyl ] -2-yl ） -1H-tetrazole 2-cyano-4 ＇-methylbiphenyl tetrazole fine chemical intermediates
分类号 TQ463 [化学工程—制药化工]
  • 相关文献

参考文献11

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  • 7[7]Spectral data of synthetic compound (1):m.p.116-117℃;[a]24 D-63(c 3,MeOH);IH NMR (400 MHz,CD3OD (δ ppm):0.77-0.90 (m,3H),0.92-0.99 (m,3H),1.00-1.12 (m,3H),1.21-1.33 (m,1H),1.35-1.43 (m,1H),1.44-1.59 (m,1H),1.63-1.67 (m,1H),2.14-2.37 (m,1H),2.49-2.55 (m,1H),2.60-2.68 (m,1H),3.30-3.34 (m,1H),4.11-4.13 (m,1H),4.57-4.79 (m,1H),7.00-7.24 (m,4H),7.50-7.62 (m,2H),7.63-7.65 (m,2H).13C NMR (100 MHz,CD3OD,δppm):14.17,19.29,19.43,20.03,20.59,23.28,23.35,28.40,28.51,29.13,34.35,34.44,47.35,50.59,64.95,67.88,124.09,124.26,127.75,128.63,128.81,128.94,129.77,130.29,131.58,131.76,132.45,138.66,138.85,139.41,139.61,143.01,143.14,156.56,156.68,172.88,173.51,176.91,177.12.MS (FAB):M+ = 435,found:436 (M++1),458 (M++Na).IR (film):3430,3116,2963,2933,2873,2745,2615,1733,1602,1472,1410,1274,1205,1163,1106,1054,998,938,853,814,759,683,623,561,519cm-1.

共引文献4

同被引文献23

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精细化工
2015年 第5期

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