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1-[4-(二甲氨基)苯亚甲基氨基]-4-苯基硫脲的合成及手性晶体结构 总被引:1,自引:0,他引:1
对二甲氨基苯甲醛和苯基氨基硫脲缩合反应生成对二甲氨基苯甲醛缩氨基苯硫脲{1-[4-(dimethylamino)ben- zylidene]-4-phenylthiosemicarbazide}, 并从溶液中析出手性晶体. 元素分析、红外光谱、紫外光谱、核磁谱、质谱和X射线衍射测定其组成和结构. 晶体属正交晶系, P212121空间群, a=0.77038(14) nm, b=1.1428(2) nm, c=1.6726(3) nm, V=1.4726(5) nm3, Z=4, Dc=1.346 g/cm3, F(000)=632, μ=0.219 mm-1, 可观测点精修最终偏离因子: R=0.0407, wR=0.1157. 化合物的晶体结构和固态圆二色谱表明化合物在结晶过程中发生单一对映体的手性堆积. 相似文献
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4—二甲氨基吡啶的合成及其催化的有机反应 总被引:11,自引:1,他引:11
综合了4-二甲氨基吡啶的制备方法及其对酰化、酯交换、烷基化等有机反应的催化作用,并探讨其在精细化工诸领域的应用前景。参考文献50篇。 相似文献
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对-二甲氨基苯甲醛和苯基氨基硫脲缩合反应生成1-[4-(二甲氨基)苯亚甲基氨基]-4-苯基硫脲(DMB), 产物能从溶液中析出单一手性对映体晶体. 用单晶X射线衍射技术测定了它的绝对构型, 晶体属正交晶系, P212121空间群, a=0.7870(2) nm, b=1.1560(2) nm, c=1.6668(3) nm, V=1.5164(5) nm3, Z=4, Dc=1.307 g/cm3, F(000)=632, μ=0.213 mm-1, 2557个可观测点[I>2s(I)]精修的最终残差因子: R=0.0409, wR=0.1061, Flack参数为0.00(9), 能够确定绝对构型. 化合物的晶体结构和大宗粉末样品的固体圆二色谱表明化合物在结晶过程中发生单一对映体的手性堆积. 相似文献
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4-二甲氨基吡啶的合成及其催化的有机反应 总被引:8,自引:0,他引:8
综述了4-二甲氨基吡啶(DMAP)的制备方法及其对酰化、酯交换、烷基化等有机反应的催化作用,并探讨其在精细化工诸领域的应用前景。参考文献50篇。 相似文献
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E. Vishnu Vardhan Reddy P. Bhanu Prakash Sandip Khobare J. Ramanatham N. Devanna 《合成通讯》2013,43(3):414-422
Novel 1-methyl-2-(2-substituted-oxazol-4-yl)-1H-benzimidazole derivatives were obtained in good yields and purity by treating corresponding 2-benzimidazolyl esters with acetamide in the presence of BF3-etherate, a Lewis acid. 相似文献
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Efficient Synthesis of (S)-3-(4-Fluorophenyl)morpholin-2-one,a Key Chiral Intermediate of Aprepitant
Song-Mei Wang 《合成通讯》2013,43(16):1871-1875
A facile, economical, and practical method for the preparation of (S)-3-(4-fluorophenyl)morpholin-2-one [(S)-9] has been developed from ethyl 2-(4-fluorophenyl)-2-oxoacetate (7) in three steps through cyclization, hydrogenation, and resolution, providing a new and convenient access to the key intermediate of antiemetic drug aprepitant. 相似文献
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Bhovi K. Venkatesh Yadav D. Bodke S. A. Biradar 《Phosphorus, sulfur, and silicon and the related elements》2013,188(9):1926-1931
A protocol for the synthesis of 3-[4-(1-benzofuran-2-yl)-1,3-thiazol-2-yl]-2-(4-aryl)-1,3-thiazolidin-4-one derivatives (5a–e) has been developed from 1-(1-benzofuran-2-yl)-2-bromoethanone (2),which served as a key intermediate for the synthesis of the title compounds. The reaction of compound 2 with thiourea furnished 4-(1-benzofuran-2-yl)-1,3-thiazol-2-amine 3, which upon further reaction with various aromatic aldehydes, gave Schiff bases 4a–e. These Schiff bases, when treated with thioacetic acid in the presence of catalytic amount of anhydrous ZnCl2, yielded thiazolidinone derivatives 5a–e. All the newly synthesized compounds have been characterized by analytical and spectral data and screened for their antimicrobial and analgesic activity. Supplemental materials are available for this article. Go to the publisher's online edition of Phosphorus, Sulfur, and Silicon and the Related Elements to view the free supplemental file. 相似文献
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The synthesis of 2-substituted isomers of the meridianins, a familiy of bioactive indole alkaloids isolated from the tunicate Aplidium meridianum, was undertaken. The synthetic route comprises six steps, with a microwave promoted Fischer cyclization as the key reaction. 相似文献
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Roland Roesler Warren E. Piers Masood Parvez 《Journal of organometallic chemistry》2003,680(1-2):218-222
The bright red title compound 1 was synthesized from (2-lithiophenyl)diphenylamine and bis(pentafluorophenyl)boron chloride. Its reactions with small acids like H2O and HCl proceeded easily giving zwitterionic compounds. For 1 and its water adduct 2 the crystal structures were determined, the latter featuring an ammonium borate structure containing a short intramolecular hydrogen bond bridge. Treatment of 1 with Jutzi's acid, [H(OEt2)2][B(C6F5)4], did not result in protonation of the nitrogen, but reaction of 1 with LiH in the presence of 12-crown-4, led to the isolation of the aminoborate [1-(Ph2N)-2-{B(H)(C6F5)2}C6H4][Li(12-crown-4)] (3). Borohydride 3 reacted with Jutzi's acid to regenerate 1 and liberate hydrogen. 相似文献
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Baichurin R. I. Reshetnikov A. A. Sergeev V. D. Aboskalova N. I. Makarenko S. V. 《Russian Journal of General Chemistry》2019,89(5):865-869
The condensation of 3-(furan-2-yl)- and 3-(thiophen-2-yl)prop-2-enals with nitro-substituted CH acids, namely ethyl nitroacetate, nitroacetone, nitroacetophenone, and nitroacetonitrile, afforded a series of geminally activated nitro dienes, 4-(furan-2-yl)- and 4-(thiophen-2-yl)-1-nitrobuta-1,3-dienes. The product structure was confirmed by NMR and IR spectroscopy.
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Krasnov V. P. Vigorov A. Yu. Nizova I. A. Grishakov A. N. Evstigneeva N. G. Kodess M. I. 《Russian Chemical Bulletin》2004,53(6):1327-1330
The reaction of dimethyl (2S,4RS)-N-phthaloyl-4-bromoglutamate with 2-methylindoline afforded diastereomeric 4-(2-methylindolin-1-yl)-(S)-glutamic acid derivatives, whose oxidation gave rise to 4-(2-methylindol-1-yl)-(S)-glutamic acid derivatives. 相似文献