共查询到18条相似文献,搜索用时 93 毫秒
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以对叔丁基苯酚为原料,经一步法制得对叔丁基杯[6]芳烃。通过逆傅克反应、亲核取代反应制得二烷基化杯[6]芳烃。最后通过磺化、亲核取代等反应,合成了下缘含喹啉基长链的新型夹状醚杯[6]芳烃化合物(2a~2c),其结构经1H NMR, 13C NMR和HR-MS(ESI-QTOF)表征。以10.0 mol%杯[6]芳烃化合物(2b)为相转移催化剂,20.0 mol%KOH为催化剂,THF为溶剂,较高产率和高选择性地合成了一系列(Z)-1,2-二芳硒基烯化合物,其结构经1H NMR和NOESY确证。2b重复使用6次,催化活性无明显降低。 相似文献
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(S)-和(R)-普萘洛尔的不对称合成 总被引:3,自引:0,他引:3
普萘洛尔是一种临床上广泛使用的β受体阻断剂, 介绍了一种不对称合成(S)-和(R)-普萘洛尔的方法. 以手性Salen-CoIII催化剂水解动力学拆分外消旋环氧氯丙烷得到高光学纯度的(S)-环氧氯丙烷和(R)-3-氯-1,2-丙二醇, 以(S)-环氧氯丙烷为手性原料先水解得(S)-3-氯-1,2-丙二醇, 其与1-萘酚反应得(S)-3-(1-萘基)-丙烷-1,2-二醇, 再与氯化亚砜反应得环状亚硫酸酯, 最后和异丙胺作用得(S)-普萘洛尔, 总收率80.9%, 光学纯度大于99%; 而同样以(S)-环氧氯丙烷为手性原料直接与1-萘酚反应得(2R)-3-(1-萘氧基)-1,2-环氧丙烷, 再与异丙胺作用得(R)-普萘洛尔, 总收率74.5%, 光学纯度大于99%. 相似文献
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3-烯-1,5-二炔是许多烯二炔类抗癌抗生素和发光材料的重要片断. 发展了一种高选择性合成E-烯二炔化合物的两步法: (1) CuBr2为卤化剂, 温和高效合成双卤代烯烃; (2)通过双卤代烯烃和末端炔烃的Sonogashira偶联反应构建烯二炔化合物. 相似文献
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通过二乙氧基硫代磷酰氯与对苯二胺反应生成了标题化合物N,N'-二(二乙氧基硫代磷酰基)-1,4-苯二胺,并应用元素分析, FTIR及1H NMR对标题化合物进行了表征. 利用X射线单晶衍射测定了其晶体结构, 同时应用TG分析法对其热性能进行了分析. 标题化合物的相对分子质量Mr=412.42, 为正交晶系, Pbca空间群, 晶胞参数为a=0.86936(16) nm, b=1.2787(2) nm, c=1.8897(3) nm, β=90°, V=2.1006(7) nm3, Z=8, Dc=1.304 g/cm3, μ(Mo Kα)=0.425 mm-1, F(000)=872, S=1.052. 最终偏离因子R=0.0628, wR=0.1860, 可观测衍射点1852个[I>2σ(I)]. 该晶体通过对苯二胺连接并以中心对称分布, 并形成层状结构, 且存在弱的分子内氢键N—H…S. TG分析表明该化合物有很好的热稳定性及成炭性, 通过其阻燃聚丙烯腈表明, 该物质是一种高效能的膨胀型阻燃剂. 相似文献
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RuiLiangLU XinHuaXU WenQiLIU QiuLinZHANG XiongCHEN 《中国化学快报》2005,16(3):325-326
Alkynyl selenide reacted with cesium arylselenolate in commercial THF at r.t under N2 to afford (Z)-1, 2-bis(arylseleno)-1-alkene in high yields. 相似文献
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Kang Bing Zou Xian Hong Yin Wen Qi Liu Ren Hua Qiu Ruo Xin Li Ling Ling Shao 《合成通讯》2013,43(14):2464-2471
In the presence of a catalytic amount of cesium hydroxide under a nitrogen atmosphere, terminal alkynes reacted with diaryl disulfides at room temperature in dimethylformamide to give almost exclusively (Z)-1,2-diarylthio-1-alkene in good yields, but under an air atmosphere, the reaction gave a mixture of alkynyl sulfide and (Z)-1,2-diarylthio-1-alkene. 相似文献
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Palimécio G. Guerrero Jr. Paulo R. de OliveiraAdriano C.M. Baroni Francisco A. MarquesRicardo Labes Gabriela R. HurtadoMiguel J. Dabdoub 《Tetrahedron letters》2012,53(39):5302-5305
An efficient and novel total synthesis of the two bioactive retinoids temarotene and arotinoid acid (TTNPB) is described. The key steps in this process include the regio and stereoselective hydrotelluration of thioacetylene 9 and Te/Li transmetalation of mixed (Z)-1,2-bis(organylchalcogene)-1-alkene (Z)-3. The subsequent reaction involving the β-phenylthio vinyl lithiated intermediate 10 with dimethyl sulfate gave the (E)-vinyl sulfide 11. The Ni+2 cross-coupling of 11 with the corresponding phenylzinc bromide and p-oxazoline phenylzinc bromide 12 afforded the respective temarotene 2 and retinoid-oxazoline substituted 13. Finally, compound 13 was deprotected with HCl to furnish arotinoid acid (TTNPB) 1. 相似文献
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In the presence of catalytic amount of cesium hydroxide the hydrothiolation of alkynyl selenides occurred at room temperature in DMF under nitrogen atmosphere to give exclusive(Z)-1-organoseleno-2-arylthio-1-alkene in excellent yields.It could provide a new and expedient way for the preparation of(Z)-1-arylseleno-2-arylthio-1-alkene. 相似文献
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Ping Tan Xianhong Yin Aihe Yu Renhua Qiu Lifen Peng Xinhua Xu Yalei Zhao Ruiren Tang 《中国化学》2011,29(4):765-768
In the presence of catalytic amount of cesium hydroxide, the hydrothiolation of alkynyl sulfides occurred at room temperature in DMF under nitrogen atmosphere to afford exclusive (Z)‐1,2‐diorganothio‐1‐alkene in excellent yields. It could provide a new and expedient way for the preparation of symmetrical and unsymmetrical (Z)‐1,2‐diorganolthio1‐1‐alkenes. 相似文献
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Md. Manzoor Hussain Mohammed Shafi G. Narayana Swamy S. G. Peeran 《Phosphorus, sulfur, and silicon and the related elements》2013,188(4):763-770
The addition of benzenethiol to p-chlorophenylphenylacetylene results in the formation of a mixture of two pairs of diastereomeric (E)- and (Z)-1-p-chlorophenyl-2-phenyl-1-phenylthioethylenes (1 and 2) and (E)- and (Z)-1-p-chlorophenyl-2-phenyl-2-phenylthioethylenes (3 and 4). The configurations of these compounds have been established by 1 H NMR studies, by their preparation from benzyl p-chlorophenyl ketone and p-chloro-benzylphenyl ketone, and by the oxidation of the thioethylenes 1, 2, 3, and 4 to the corresponding sulphonylethylenes 5, 6, 7, and 8, respectively. 相似文献