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2,8-二氨基-10-甲氧基-5,10-二氢磷杂吖嗪-10-氧化物的合成、诱变性及应用性能研究 总被引:6,自引:0,他引:6
10-羟基-5,10-二氢磷杂吖嗪-10-氧化物(1)经酰氯化、甲基化得到10-甲氧基-5,10-二氢磷杂吖嗪-10-氧化物(2),2经硝化得到10-甲氧基-2,8-二硝基,5,10-二氢磷杂吖嗪-10-氧化物(3.62%).3在Pd/C(u=0.05)存在下,用氢气还原为2,8-二氨基-10-甲氧基-5,10-二氢磷杂吖嗪-10-氧化物(4.71%),考察了Bd/C(w=0.05)用量对氢化还原反应的影响.经过Salmonella/mammalian microsome assay测试,4表现为非诱变性,用4与乙酰J-酸作用得到新型双偶氮酸性染料(5).5对羊毛和丝绸分别在2%与3%色度下浸染郜得到黑色染样,考察了5的上染曲线,并对染样进行了测色研究,发现该染料属于酸性蓝黑染料,其黑度优于目前市场上流行的酸性黑10B. 相似文献
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YIN zhi-gang ZHAO De-feng 《高等学校化学研究》2003,19(1):32-36
Ph2NH and PCl3 interacted at a molar ratio of 1:1.05 and slow-elevated temperature and then at 210-220 ℃ for 6h.The brown solution obtained was treated with H2O to produce a very hard brown solid believed to be a mixture of 5,10-dihydrophenophosphazine 10-oxide(1a) and 10,10′(5H,5H′)-spirobipenophosphazinium chloride(1b).This brown solid was directly oxidized with peracetic acid in HOAc prior to the separation of them to give compound 10-hydroxy-5,10-dihydropheno-phosphazine 10-oxide(2) with a higher yield(45%) than that of the literature(27%).When treated with excess SOCl2.compound 2 could quantitatively be converted to the corresponding phosphinyl chloride and the latter could further be transformed into 10-methoxy-5,10-dihydrophenophosphazine 10-oxide in 70% as treated with NaOMe in methanol.Compound 2 could also be converted to a bisanion when treated with NaH in DMF.The resulted bisanion reacted with MeI to give 5-methyl-10-hydroxy-5,10-dihydrophenophosphzine 10-oxide in a 73% yield which would be converted to 5-methyl-10-methoxy-5,10-dihydrophenophosphazine 10-oxide.All these compounds obtained were identified by surveying their melting points.and spectra and elemental analysis. 相似文献
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2-氨基-10-羟基-5,10-二氢磷杂吖嗪-10-氧化物的合成、诱变性及应用 总被引:3,自引:0,他引:3
2-氨基-10-羟基-5;10-二氢磷杂吖嗪-10-氧化物的合成、诱变性及应用;二氢磷杂吖嗪; 吡唑啉酮; 合成; 结构鉴定; 诱变性 相似文献
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A New Technique of Synthesizing 10—Hydroxy—5—methyl—5,10—dihydrophenophosphazine 10—Oxide 总被引:1,自引:0,他引:1
ZhiGangYIN DeFengZHAO 《中国化学快报》2003,14(4):347-350
10-Hydroxy-5-methyl-5,10-dihydrophenophosphazine 10-oxide(1)was prepared by a new technique of treating 10-methoxy-5,10-dihydrophenophosphazine 10-oxide(2)with an equivalent of NaH in anhydrous DMF,and then at 120℃ for 3-4h,which not only avoided poisonous and expensive methyl iodide used in literature,but made the consumption of NaH greatly decrease as well.The possible reaction mechanism was also described.The chemical structure of 1 was confiremed by IR,NMR,and mass spectroscopy. 相似文献
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2,8-二氨基-10-羟基-5-甲基-5,10-二氢磷杂吖嗪-10-氧化物的合成及其诱变性研究 总被引:3,自引:0,他引:3
在升温条件下,二苯胺和三氯化磷反应,产物经水解、氧化得次膦酸:10-羟基-5,10-二氢磷杂吖嗪-10-氧化物(产率45%).经酰化后,与甲醇钠作用,生成相应的次膦酸甲酯.次膦酸甲酯经NaH处理后,在120℃下发生甲基迁移,形成5-甲基次膦酸(产率62%).用45倍摩尔量的硝化剂将5-甲基次膦酸硝化,得到双硝基产物(产率59%).在5%Pd/C催化下,双硝基产物又被氢气还原.考察催化剂用量对该还原反应的影响,并在最佳催化剂用量时得到2,8-二氨基-10-羟基-5-甲基-5,10-二氢磷杂吖嗪-10-氧化物(产率70%).用NMR,IR和质谱确定了所合成的5个中间体结构.对合成的氨基化合物进行Salmonella/mam-malianmicrosomeassay测试,结果表明,该氨基化合物表现为非诱变性. 相似文献
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合成了N-(1-甲基-4,5-二溴-2-三氯乙酰基)甘氨酸甲酯(C9H10Br2N2O3,
Mr=354.01),X-射线单晶衍射确定其属于正交晶系,P2(1)2(1)2(1) 空间群,
a=6.4237(18)(A), b=13.445(4)(A), c=14.054(4)(A), α=β=γ= 90°, V=1213.8(6)(A)3, Z=4,
Dc=1.937 Mg·m3, μ=6.672 mm-1, F(000)=688.有2257个可观察点[I>2σ(I)],最终R1=0.0275,
wR2=0.0682.X-射线晶体结构的分析表明该化合物含羰基、酰胺基、酯基与溴原子,并且通过N(2)H与O(2)分子间氢键连成一维链状结构. 相似文献
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1 INTRODUCTION The sulfonylurea herbicides are characterized by broad-spectrum weed control at very low use rates (c.2~75g ai ha-1), good crop selectivity and very low acute and chronic animal toxicity (acute oral LD50 to rat >4000 mg/kg)[1]. They are e… 相似文献
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Nickel-basedcatalystsarewidelyusedinthechemicaliridustry,suchasinhydrogenation,steamreforming,andmethanationreactions1.Thecatalyticperformancesofnickelcatalystsaresensitivetopreparationmethods,supportsandpromoters=.ThecatalyticconversionofmethylformatetomethylacryIateisaveryinterestingprocess,inwhich,viamethyIformate,thetranspoFtandhand1ingCO/CH,OHatlocationswherethelatteraredifficulttoobtainortohandlecanbesimplified'.Nickel-basedcatalystswerepreparedbywetimpregnationusingoneofNi(NO,),,Ni… 相似文献
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1INTRODUCTIONInorganicsolidsupportsascatalystshavebeenwellstudied,becauseoftheirap-plicationsinorganicsynthese('~".Recently,wehavereportedtheKnoevenagelcon-densationcatalysedbyKF-Al,O,['i.Inthispaper,wediscussedthecrystalstruc-tureofthetitlecomPoundsynthesizedbythereactionof2-chlorobenzaldehydey5,5-dimethyl-1,3-cyclohexanedioneandisopropylidenemalonateinmethanolcatalyzedbyKF-Alzo,'Inordertoconfirmthestructureofthetitlecompound,theX-raycrys-tallOgraphicstudywascarriedout.2EXPER1MEN… 相似文献
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Yosuke Sato Chihiro Takagi Prof. Dr. Ryo Shintani Prof. Dr. Kyoko Nozaki 《Angewandte Chemie (International ed. in English)》2017,56(31):9211-9216
A palladium-catalyzed asymmetric synthesis of silicon-stereogenic 5,10-dihydrophenazasilines was developed that proceeds via an unprecedented enantioselective 1,5-palladium migration. High enantioselectivity was achieved by employing 4,4′-bis(trimethylsilyl) (R)-Binap as the chiral ligand, and a series of mechanistic investigations were carried out to probe the catalytic cycle of this process. 相似文献
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PAN Ying-Minga ZHANG Yea WANG Heng-Shana② CHEN Zhen-Fenga WU Qianga GE Chun-Yua ZHANG Yongb a 《结构化学》2006,25(10):1209-1212
1 INTRODUCTION Pine resin is a very abundant renewable natural source mainly composed of diterpenic resin acids with the general formula C19H29COOH, which has been widely applied in industrial manufactures and fine chemicals[1]. Recently, a series of research re- sults show that the resin acid derivatives are poten- tially useful intermediates in the synthesis of drugs active against viruses[2~5]. Their antiviral activity and function as nucleoside analogues or non- nucleoside inhibito… 相似文献
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1-苯基-3-甲基-4-苯甲酰基-5-吡唑啉酮(HPMBP)缩甘氨酸甲酯的合成、表征和晶体结构 总被引:4,自引:0,他引:4
合成了化合物1-苯基-3-甲基-4-苯甲酰基-5-吡唑啉酮(HPMBP)缩甘氨酸甲酯,用红外光谱、核磁共振谱和元素分析等方法进行了表征,用X射线衍射方法测定了其晶体结构.晶体学参数如下:三斜晶系,空间群为P1, a=0.9403(3) nm, b=0.9884(3) nm, c=1.0127(3) nm, α=86.666(7)°, β=89.827(6)°, γ=73.951(6)°, V=0.9029(5) nm3, Z=2, Dc=1.285 Mg·m-3, μ=0.088 mm-1, F(000)=368.最终偏离因子R1=0.0452, wR2=0.0889. 相似文献
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甲基迁移反应在合成化学和生命科学领域具有重要意义.迄今为止,所报道的甲基迁移反应大多数发生在不同种类分子之间.因此,寻找新型甲基迁移反应具有一定的研究价值.本研究以环境中常见的杀虫剂倍硫磷为研究对象,采用电喷雾质谱技术为分析工具对反应体系进行高灵敏分析,探究在CF3COOH及纳米二氧化钛(TiO2)条件下,倍硫磷分子中发生甲基迁移反应的可能性.结果表明,在CF3COOH和TiO2共同作用下,倍硫磷分子中的甲基可以从同一分子的氧原子上迁移到不饱和硫原子上,发生分子内1,3-甲基迁移反应,形成异构体硫甲基化产物;同时,异构体产物中的甲基还可以从硫原子上再继续迁移到另一分子倍硫磷的不饱和硫原子上,发生分子间甲基迁移反应.同时结合密度泛函理论计算对倍硫磷分子内和分子间甲基迁移反应的过程进行动态模拟,并对其迁移机理进行解释.本研究发现了倍硫磷能发生分子内和分子间甲基迁移反应,提供了一种研究甲基迁移反应的质谱方法,为倍硫磷的降解研究提供了新思路. 相似文献
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环丙基甲基酮是合成环丙氟哌酸类广谱抗菌药物和抗艾滋特效药依法韦仑的重要中间体,在医药、化工及农林等领域均有广泛应用。环丙基甲基酮的合成方法大致分为4类,分别以酮类、酯类、醇类及呋喃有机物为原料,在一定条件下生成环丙基甲基酮粗品,经萃取及精馏得到环丙基甲基酮纯品。本文综述了环丙基甲基酮的合成研究进展。 相似文献