O－烷基，O－芳基硫代磷酰取代硫脲和O－烷基硫代磷酰－双－取代硫脲的研究（Ⅱ）

用硫氰酸钾与硫代磷酰氯制备了硫代磷酰异硫氰基酯和二异硫氰基酯，并以其与不同胺反应，合成了硫代磷酰取代硫脲和硫代磷酰－双－取代硫脲两系列２０个新的有机磷化合物，经~１ＨＮＭＲ、ＩＲ及元素分析确定了它们的化学结构，测定了它们的生物活性。结果表明只有Ｏ－异丙基，Ｏ－（４－甲基－２－硝基苯基）－Ｎ＇－萘基硫代磷酰硫脲（ＰＤ－１）具有较好的杀菌活性。     

O—烷基苯基硫代磷酰取代硫脲的合成（Ⅲ）：含P—C键化合物的…

利用Ｏ－烷基苯基硫代磷酸酸异硫氰基酯与胺与胺的加成反应，合成了两系列Ｏ－烷基苯基硫代磷酰取代硫脲化合物，经元素分析、ＩＲ和＾１ＨＮＭＲ确定了它们的结构，并进行了除草活性的测试。     

O-乙基-N-烷基(取代硫脲基)硫代磷酰胺酯的合成及其生物活性

采用O-乙基-N-烷基(异硫氰基)硫代磷酰胺酯与不同胺的加成反应,合成了一系列新型的O-乙基-N-烷基(取代硫脲基)硫代磷酰胺酯,其结构经元素分析、IR及¹HNMR证实.生物活性初步测定表明,这类化合物均具有一定的广谱杀菌及除草活性.     

O-烷基苯基硫代膦酰取代硫脲的合成(Ⅲ)──含P─C键化合物的研究

利用O-烷基苯基硫代膦酸异硫氰基酯与胺的加成反应,合成了两系列O-烷基苯基硫代膦酰取代硫腺化合物。经元素分析、IR和¹NNMR确定了它们的结构,并进行了除草活性的测试。     

O-烷基,O-芳基硫代磷酰取代硫脲和O-烷基硫代磷酰-双-取代硫脲的研究

通过O-烷基,O-芳基硫代磷酸异硫氰基酯和O-烷基硫代磷酸二异硫氰基酯与不同胺的加成,合成了通式为:的两系列有机磷化合物。这些化合物在文献中均未见报道。初步生物测试结果表明,它们都具有一定的除草活性,其中个别化合物有较高的除草活性。产物和中间体结构经红外光谱和核磁共振谱鉴定。并对合成中的一些问题进行了初步探讨。     

N，N＇－硫代磷酰基芳酰胺基硫脲的合成及生物活性

Ｎ，Ｎ＇－硫代磷酰基芳酰胺基硫脲的合成及生物活性金桂玉，解敏雨，赵国锋（南开大学元素有机化学研究所天津３０００７１）关键词芳酰肼，硫代磷酰基异硫氰酸酯，硫代磷酰基芳酰胺基硫脲，合成，生物活性含（硫代）磷酰基的硫脲衍生物具有广泛生物活性，如杀虫［１，２...     

6-取代苯并噻唑-2-氨基硫代磷酸二烷基酯的合成

用6-位取代的2-氨基苯并噻唑与三氯硫磷反应,合成了3个苯并噻唑-2-氨基硫代磷酰二氯,并由此合成了9个苯并噻唑-2-氨基硫代磷酸二烷基酯.讨论了苯并噻唑环上取代基对反应的影响和产物中硫代磷酸酯的烷基的空间效应对反应的影响.所合成的部分化合物对人喉鳞状细胞癌(Hep-2)具有一定的抑制能力.     

O-乙基-N-异丙基(取代硫脲基)硫代磷酰胺酯类衍生物杀菌作用的构效关系研究

研究了一系列O-乙基-N-异丙基(取代硫脲基)硫代磷酰胺酯类化合物的杀菌活性,发现分子的活性中心在硫脲基上,其氮原子上所连的取代基对活性有重要影响。采用取代基物理参数及化合物对多种植物病菌的抑制活性,进行了结构与活性定量关系的研究。建立了较好的结构与活性的相关式,预测出更高活性的化合物并得到实验证实。     

应用FTIR光谱研究不同取代苯胺对O－乙基－N－异丙基（取代硫脲基）硫代磷酰胺酯生成反应的影响

应用ＦＴＩＲ光谱研究不同取代苯胺对Ｏ－乙基－Ｎ－异丙基（取代硫脲基）硫代磷酰胺酯生成反应的影响何兰龄，赖城明，林，徐谨民，王永泰，杨华铮，吴烨（南开大学化学系，天津，３０００７１）（南开大学中心实验室）（南开大学元素有机化学研究所）关键词ＦＴＩＲ，取...     

硫代磷酰脲衍生物的研究 VI: N-(O-烷基-O-芳基硫代磷酰基)-N''-芳酰基脲

用硫代磷酰胺酸与芳酰基异氰酸酯的亲核加成合成了32个N-(O-烷基-O-芳基硫代磷酰基)-N'-芳酰基脲类化合物, 并用元素分析 , 红外光谱, 质子核磁共振和质谱表征了这些化合物的结构.     

硫代磷(膦)酰基脲类衍生物的合成及其生物活性

通过O,O-二乙基硫代磷酰基异氰酸酯或O-乙基-苯基硫代膦酰基异氰酸酯与不同胺的加成反应,合成了一系列新型硫代磷(膦)酰基脲类化合物,其结构经元素分析、¹HNMR及MS确证。初步的生物活性测定表明,这类化合物具有一定的除草、抗肿瘤及抑制几丁质形成活性。     

酪胺的磷(膦)酰化反应及其衍生物合成的研究

本文合成了O-烷基(或O-取代苯基)-O-烷基(或苯基)-N-(对-羟基-β-苯乙胺基)硫代磷(膦)酰胺酯及O,N-双[O-烷基(或O-取代烷基)-O-烷基(或苯基)硫代磷(膦)酰基]对-羟基-β-苯乙胺32个新化合物,讨论了氮优先磷酰化,研究了不同碱的催化机理及磷(膦)酰化试剂对酪胺反应选择性差别。通过元素分析、IR、1H NMR及MS证明了结构。生物初筛表明部分化合物有杀虫活性。     

The Reactions of 1-Acetothiosemicarbazidc with P(NR_2)_3 PC1_3 and PCI_5

A Series of new heterocyciophosphorus compounds were synthesizec oy cyclocondensa-tion of 1-acetothiosemicarbazide with P(NR2)3. The further reaction of these compounds with P(NR2)3 gave different compounds depending upon different reaction conditions. The 1-acetothiosemicarbazide can also condense with PCl3 and PCl5 similarly, The reaction mechanism, the spectral properties and chemical properties of these products were also studied and discussed.     

Synthesis and Characterization of Ferrocene Derived Cyclic Carbaphosphazenes

Dialkylamino substituted cyclic carbaphosphazenes, (R 2 NCN) 2 (NPCl 2 ) were prepared and reacted with the ferrocene derived hydroxymethyl phosphine sulfide FcCH(CH 3 )P(S)(CH 2 OH) 2 after dilithiation to yield a series of new spirocyclic derivatives of cyclic carbaphosphazenes having ferrocenyl pendant groups. To confirm the formation of six membered spirocycles and to compare their spectral features, transesterification reactions of FcCH(CH 3 )P(S)(CH 2 OH) 2 also were carried out with P(NR 2 ) 3 , yielding the six membered heterocycles FcCH 2 P(S)(CH 2 O) 2 PNR 2 (R = Me, Et). The compounds were characterized by 1 H, 31 P, 13 C NMR, mass spectra, and elemental analysis.     

Synthesis and Characterization of Dichlorotin(IV)trithiophosphates and Their Adducts with Nitrogen Donor Bases

Abstract

Dichlorotin(IV)trithiophosphates [(RO)P(S)S ₂ ]SnCl ₂ were prepared by the reaction of methanolic solution of SnCl ₄ and dipotassium salt of trithiophosphates in a 1:1 molar ratio and their adducts [(RO)P(S)S ₂ ]SnCl _2.N ₂ C ₁₂ H ₈ and [(RO)P(S)S ₂ ]SnCl _2.N ₂ C ₁₀ H ₈ were prepared by the reaction of methanolic solution of [(RO)P(S)S ₂ ]SnCl ₂ and N-donor bases in a 1:1 molar ratio. These newly synthesised derivatives have been characterized by elemental analysis; molecular weight measurements; and IR, ¹³ C, ³¹ p and ¹¹⁹ Sn NMR spectral studies. Coordination number of four and six was suggested for dichlorotin (IV)trithiophosphates and their adducts with N-donor bases respectively.     

Perfluoroalkyl(dithiocarbamato) tellurium(II) compounds

[NMe(4)][R(f)Te(SC(S)NR(2))(2)] derivatives are selectively formed by the oxidation of [NMe(4)]TeR(f) (R(f) = CF(3), C(2)F(5)) with [R(2)NC(S)S](2) (NR(2) = NEt(2), NBz(2), N(CH(2))(4)) in almost quantitative yields. An alternative route to obtain the dithiocarbamato complex anions offer reactions of Te[SC(S)NR(2)](2) (NR(2) = NEt(2), NBz(2)) with equimolar amounts of Me(3)SiR(f) and [NMe(4)]F. Some of the derivatives were recrystallized with bulky cations in order to determine the crystal structures. Structural elucidation by diffraction methods exhibit the structural feature of a distorted pentagonal planar environment (resembling "butterflies") around the tellurium centres. The carbamato tellurates can be transferred easily into the neutral derivatives, R(f)TeSC(S)NR(2), upon treatment with Ag[BF(4)]. In solution they equilibrate with Te(2)(R(f))(2) and [R(2)NC(S)S](2) and finally are transformed into Te(R(f))(2), Te[SC(S)NR(2)](2), and Te[SC(S)NR(2)](4), respectively. All compounds are fully characterized by NMR spectroscopic methods ((1)H, (13)C, (19)F, (125)Te). Additionally, synthesis and characterization of the hitherto unknown derivative [NMe(4)]TeC(2)F(5) are described.     

Synthese von N-Di(alk-, ar-)oxyphosphoryl-tri(alk-, ar-)-oxyphosphazenen, (RO)2P(O)?NP(OR)3, durch P?N-Bindungsknüpfung

Synthesis of N-Di(alk-, ar-)oxyphosphoryl-tri(alk-, ar-)oxyphosphazenes, (RO)₂P(O)? N?P(OR)₃, by P? N-Bond Formation The title compounds can be prepared from di- and triesters of phosphorous acid, sodium azide, and carbon tetrachloride in a single step procedure and in high yields. Due to the combination of the Atherton-Todd and the Staudinger reaction toxic phosphoric acid ester azides are formed only in situ and their concentration is kept very small. As by-products trichloromethane phosphonic acid esters, (RO)₂P(O)CCl₃, esters of phosphoric acid and condensed phosphoric acids as well as N-alkylimidodiphosphoric acid esters, [(RO)₂P(O)]₂NR, are formed. Their formation can be avoided or reduced by choosing suitable reaction conditions. The mechanism of the reaction is discussed.