Synthesis, Structure and Dielectric Property of Ba_(1- x)Sr_xZr_yTi_(1- y)O_3

ＩｎｔｒｏｄｕｃｔｉｏｎＢａＴｉＯ３ｉｓａｓｔｒｏｎｇｄｉｅｌｅｃｔｒｉｃｍａｔｅｒｉａｌ，ｗｈｉｃｈｉｓｗｉｄｅｌｙｕｓｅｄｉｎｔｈｅｐｒｏｄｕｃｔｉｏｎｏｆｅｌｅｃｔｒｉｃｃｏｍｐｏｎｅｎｔｓｓｕｃｈａｓｃｅｒａｍｉｃｃａｐａｃｉｔｏｒ，ＰＴＣ，ｍｅｄｉｕｍａｍｐｌｉｆｅｒ［１］．Ｉｔｈａｓｔｈｅｈｉｇｈｅｓｔｄｉｅｌｅｃｔｒｉｃｃｏｎｓｔａｎｔａｔ１２０℃（ｃａ．１０４），ｗｈｉｌｅｉｔｓｄｉｅｌｅｃｔｒｉｃｃｏｎｓｔａｎｔａｔｒｏｏｍｔｅｍｐｅｒａｔｕｒｅｉｓｏｎｌｙ１／６ｏｆｔｈｅＣｕ…     

Synthesis and Structure of Copper(Ⅱ) Complex [Cu(C_5H_5N)_2(H_2O)(C_6H_5COO)_2]

1　ＩＮＴＲＯＤＵＣＴＩＯＮＣｅｒｔａｉｎｃｏｐｐｅｒｃｏｍｐｌｅｘｅｓｈａｖｅｂｅｅｎｓｈｏｗｎｔｏｈａｖｅｕｎｕｓｕａｌｃｈｅｍｉｃａｌｐｒｏｐｅｒｔｉｅｓｓｕｃｈａｓｏｘｙｇｅｎｔｒａｎｓｆｅｒ,ｏｘｉｄａｔｉｖｅａｄｄｉｔｉｏｎａｎｄｈｏｍｏｇｅｎｏｕｓｃａｔａｌｙｔｉｃｈｙｄｒｏｇｅｎａｔｉｏｎ[1].Ｏｘｉｄａｔｉｖｅａｄｄｉｔｉｏｎｒｅａｃｔｉｏｎｓａｒｅｋｅｙｓｔｅｐｓｉｎｔｈｅａｃｔｉｖａｔｉｏｎｏｆσｂｏｎｄｓｉｎａｇｒｅａｔｎｕｍｂｅｒｏｆｃａｔａｌｙｔｉｃｐｒｏｃｅｓｓ.Ｃｏｐ…     

Synthesis and Crystal Structure of H_2Mo_8O_(26)〔(n-Bu)_4N_2〔(CH_3)_2 COHCH_2COCH_3〕_2

1　ＩＮＴＲＯＤＵＣＴＩＯＮＰｏｌｙｍｏｌｙｂｄａｔｅａｎｉｏｎｓｈａｖｅｂｅｅｎｓｔｕｄｉｅｄｆｏｒｍａｎｙｙｅａｒｓｂｅｃａｕｓｅｏｆｔｈｅｉｒａｐｐｌｉｃａ ｔｉｏｎｉｎｃａｔａｌｙｓｉｓｃｈｅｍｉｓｔｒｙ〔1〕.Ｉｎｔｈｅｓｙｎｔｈｅｓｉｓｏｆｏｒｇａｎｉｃｐｏｌｙｍｏｌｙｂｄａｔｅｄｅｒｉｖａｔｉｖｅｓｕｓｉｎｇａｃｅｔｏｎｅａｓｓｏｌｖｅｎｔ,ｗｅｆｏｕｎｄｔｈａｔｔｈｅｃｏｎｄｅｎｓａｔｉｏｎｒｅａｃｔｉｏｎｏｆａｃｅｔｏｎｅｏｃｃｕｒｒｅｄａｎｄｔｈｅｃｏｎｄｅｎｓａｔｉｏｎｐｒｏｄ…     

Study on the Crystal Structure of RS-1-(2-methoxyphenyl)-4-〔3-(1-naphthyloxy)-2-hydroxypropyl〕-piperazine

ＩＮＴＲＯＤＵＣＴＩＯＮＮａｆｔｏｐｉｄｉｌ，ＲＳ １ （２ ｍｅｔｈｏｘｙｐｈｅｎｙｌ） ４ 〔３ （１ ｎａｐｈｔｈｙｌｏｘｙ） ２ ｈｙｄｒｏｘｙｐｒｏｐｙｌ〕 ｐｉｐｅｒａｚｉｎｅ，ｉｓａｎｏｖｅｌａｎｔｉｈｙｐｅｒｔｅｎｓｉｖｅｄｒｕｇｃｕ...     

Synthesis,Characterization and Crystal Structure of〔Co_2Mo_2(μ-_4-C_2HPh)(μ-CO)_4(CO)_4(η~-5C_5H_4C(O)Me)_2〕

１　ＩＮＴＲＯＤＵＣＴＩＯＮＤｉｍｏｌｙｂｄｅｎｕｍａｌｋｙｎｅｃｏｍｐｌｅｘｅｓ〔Ｍｏ２（μＲ１Ｃ≡ＣＲ２）（ＣＯ）４（η５Ｃ５Ｈ５）２〕ｃａｎｒｅａｃｔｗｉｔｈａｖａｒｉｅｔｙｏｆｒｅａｇｅｎｔｓｓｕｃｈａｓｐｈｏｓｐｈｉｎｅｓ,ｔｈｉｏｌｓ,ｅｌｅｍｅｎｔａｌｓｕｌｆｕｒ,Ｒｕ３（ＣＯ）１２ａｎｄＣｏ２（ＣＯ）８〔１－４〕．Ｉｎｔｈｅｐｒｏｄｕｃｔｓｔｈｅａｌｋｙｎｅｌｉｇａｎｄｉｓｕｓｕａｌｌｙｒｅｔａｉｎｅｄ．Ｓｏｍｅｔｉｍｅｓ,ａｌｋｙｎｅｓｃｉｓｓｉｏｎｏｃｃｕｒｓ．Ｂｅｉｎｇ…     

Synthesis and Structural Characterization of Two Molybdenum~phosphate Cluster Compounds: (C_(14)N_(14)H_(63) )Na(H_2Mo_6P_4O_(31))_2·8H_2Oand(C_(14)N_(14)H_(63))Na(H_2Mo_6P_4O_(31) )_2·5H_2O

ＩｎｔｒｏｄｕｃｔｉｏｎＴｈｅｓｙｎｔｈｅｓｉｓａｎｄｓｏｒｐｔｉｏｎｐｒｏｐｅｒｔｉｅｓｏｆｏｐｅｎｆｒａｍｅ ｗｏｒｋｓｏｌｉｄｓｓｕｃｈａｓｚｅｏｌｉｔｅｓ1ａｎｄｍｅｔａｌｍｏｌｙｂｄｅｎｕｍｐｈｏｓ ｐｈａｔｅ2 ,3ｗｉｔｈｌａｒｇｅｃａｖｉｔｉｅｓｐｒｏｖｏｋｅｄｅｎｏｒｍｏｕｓｉｎｔｅｒｅｓｔｂｅ ｃａｕｓｅｏｆｔｈｅｉｒｐｏｔｅｎｔｉａｌａｐｐｌｉｃａｔｉｏｎｉｎｃａｔａｌｙｓｉｓ .Ｏｎｅ ,ｔｗｏ ａｎｄｔｈｒｅｅ ｄｉｍｅｎｓｉｏｎａｌｓｏｌｉｄｃｏｍｐｏｕｎｄｓｃｏｎｓｉｓｔｉｎｇｏ…     

Synthesis and Crystal Structure of〔( PPh_3)( CH_3 COS) _2 NiB_(10) H_(10)〕·0 .4( C_5 H_(12))

１　ＩＮＴＲＯＤＵＣＴＩＯＮＷｅｈａｖｅｓｈｏｗｎａｎｉｎｔｅｒｅｓｔｉｎｅｘｏｐｏｌｙｈｅｄｒａｌｃｙｃｌｉｚａｔｉｏｎｏｆｍｅｔａｌｌｉｇａｎｄｓｔｏｃｌｕｓｔｅｒ．ＡｓｅｒｉｅｓｏｆｍｅｔａｌｌａｂｏｒａｎｅｃｏｍｐｏｕｎｄｓｃｏｎｔａｉｎｉｎｇｆｉｖｅｍｅｍｂｅｒｅｄｒｉｎｇｓｓｕｃｈａｓＭ－Ｏ－Ｃ－Ｏ－ＢａｎｄＭ－Ｓ－Ｃ－Ｏ－Ｂａｒｅｓｙｎｔｈｅｓｉｚｅｄａｎｄｃｈａｒａｃｔｅｒｉｚｅｄ．Ｔｈｅｇｒｏｕｐｓｏｆｃｙｃｌｉｚａｔｉｏｎｉｎｃｌｕｄｅａｃｅｔａｔｅ〔１〕,ｂｅｎｚｏａｔ…     

Solid State Synthesis and Structural Characterizationof Binuclear Cu( I)-Sb Ph_3 Co m plex 〔 Cu( Sb Ph_3)_2 I〕

１　ＩＮＴＲＯＤＵＣＴＩＯＮＣｕ（Ｉ）ｃｏｍｐｌｅｘｅｓｗｉｔｈｐｈｏｓｐｈｉｎｅａｎｄａｒｓｉｎｅｌｉｇａｎｄｓａｒｅｗｅｌｌｋｎｏｗｎ〔１〕．ＦｏｒＣｕｐｈｏｓｐｈｉｎｅｃｏｍｐｌｅｘｅｓ，ｔｈｅＣｕ∶ｌｉｇａｎｄｒａｔｉｏｖａｒｉｅｓｆｒｏｍ１∶１ｔｏ１∶４ａｎｄｃｏｏｒｄｉｎａｔｉｏｎｇｅｏｍｅｔｒｙｏｆＣｕ（Ｉ）ｒａｎｇｅｓｆｒｏｍｌｉｎｅａｒｔｏｔｒｉｇｏｎａｌ，ｔｈｅｎｔｏｔｅｔｒａｈｅｄｒａｌｅｘｔｒｅｍｅｓ；ｆｏｒｅｘａｍｐｌｅ，ｔｈｅ１∶２ａｄｄｕｃｔｓＣｕ（ＰＰｈ３）…     

Synthesis and Crystal Structure of Monochloridehepta(dimethyl sulfoxide)gadolinium(Ⅲ) di(tetraphenyl boron) Salt 〔Gd(dmso)_7Cl〕〔BPh_4〕_2

１　ＩＮＴＲＯＤＵＣＴＩＯＮＳｕｌｆｏｘｉｄｅｉｓｋｎｏｗｎｔｏｆｏｒｍｃｏｏｒｄｉｎａｔｉｏｎｃｏｍｐｏｕｎｄｓｗｉｔｈＬａｎｔｈａｎｉｄｅ（Ⅲ）ａｎｄｔｈｅｉｒｓｙｎｔｈｅｓｅｓ,ｐｒｏｐｅｒｔｉｅｓａｎｄｖａｒｉｏｕｓｐｈｙｓｉｃａｌｃｈａｒａｃｔｅｒｉｓｔｉｃｓｈａｖｅｂｅｅｎｒｅｐｏｒｔ－ｅｄ〔１～９〕．Ｈｏｗｅｖｅｒ,ｔｈｅｒｅａｒｅｓｏｍａｎｙｄｉｆｆｉｃｕｌｔｙｉｎｐｒｅｐａｒｉｎｇｔｈｅｋｉｎｄｏｆｌａｎｔｈａｎｉｄｅｃｏｍｐｌｅｘｅｓｂｅｃａｕｓｅｔｈｅａｎｉｏｎｓｕｓｅｄａ…     

Preparation, Characterization of Solid SolutionLa_4BaCu_(5- x)Mn_xO_(13 λ)(x= 0—5) and ItsCatalytic Activity in the Reduction of NO by CO

ＩｎｔｒｏｄｕｃｔｉｏｎＴｈｅｄｉｓｃｏｖｅｒｙｏｆｔｈｅｓｕｐｅｒｃｏｎｄｕｃｔｉｖｉｔｙｏｆｔｈｅＢａ－Ｌａ－Ｃｕ－Ｏｓｙｓｔｅｍａｔｈｉｇｈｔｅｍｐｅｒａｔｕｒｅｓｈａｓｇｒｅａｔｌｙｓｔｉｍｕｌａｔｅｄｔｈｅｉｎｖｅｓｔｉｇａｔｉｏｎｏｆｃｕｐｒａｔｅｓ［１］．Ｃｕｐｒａｔｅｓｈａｖｅｂｅｅｎｆｏｕｎｄｔｏｂｅａｃｔｉｖｅｃａｔａｌｙｓｔｓｆｏｒｓｅｖｅｒａｌｒｅａｃｔｉｏｎｓ，ｉｎｃｌｕｄｉｎｇｔｈｅｒｅｄｕｃｔｉｏｎａｎｄｄｅｃｏｍｐｏｓｉｔｉｏｎｏｆＮ２Ｏ，ＮＯａｎｄＮＯ２，ｔｈｅ…     

(S)-(-)-5-对苄氧基苄基-2,4-噁唑烷二酮的合成

L-酪氨酸经O-苄基化和重氮化反应得到关键中间体--手性3-(对苄氧基苯基)-α-羟基丙酸(4); 4经酯化、氨化和环化反应合成了(S)-(-)-5-对苄氧基苄基-2,4-噁唑烷二酮,总收率10%, 95.4%e.e.,其结构经1H NMR和HR-MS表征.     

(S)-(-)-norlaudanosine和(S)-(-)-O,O-dimethylcoclaurine的合成

以高藜芦胺为起始原料,经N-磺酰化反应制得高藜芦磺酰胺(2);2分别与芳乙烯甲醚经对甲苯磺酸催化的Pictet-Spengler反应后用金属钠脱除Ts基团合成了(±)-norlaudanosine(5a)和(±)-O,O-dimethylcoclaurine(5b);使用半量拆分法,以N-乙酰-L-苯丙氨酸为拆分剂,制得(S)-(-)-5a和(S)-(-)-5b,其结构经1H NMR,13C NMR,IR,MS和HR-ESI-MS确证。     

Preparation,molecular structures,and characteristic properties of (E)-1-(2-furyl)- and (E)-1-(2-thienyl)-2-(3-guaiazulenyl)ethylenes and (E)-1-(3-furyl)- and (E)-1-(3-thienyl)-2-(3-guaiazulenyl)ethylenes

Wittig reactions of 2-furaldehyde (20) [and thiophene-2-carbaldehyde (21)] with (3-guaiazulenylmethyl)triphenylphosphonium bromide (19) in ethanol containing NaOEt at 25 °C for 24 h under argon give (E)-1-(2-furyl)-2-(3-guaiazulenyl)ethylene (22E) and (E)-1-(2-thienyl)-2-(3-guaiazulenyl)ethylene (23E) in 53 and 36% yields. Similarly, Wittig reactions of 3-furaldehyde (29) [and thiophene-3-carbaldehyde (30)] with 19 under the same reaction conditions as for 20 and 21 afford (E)-1-(3-furyl)-2-(3-guaiazulenyl)ethylene (31E) and (E)-1-(3-thienyl)-2-(3-guaiazulenyl)ethylene (32E) in 32 and 46% yields. Molecular structures and characteristic properties as well as preparation of the title E (i.e., one of the geometrical isomers) forms, with a view to comparative study, are reported. Moreover, reactions of those conjugated π-electron systems with TCNE (=tetracyanoethylene) in benzene [and in DMF (=N,N-dimethylformamide)] at 25 °C for 24 h under argon yield unique products, possessing interesting molecular structures, respectively, whose characteristic properties and crystal structures are documented, also.     

Synthesis and Crystal Structure of 1-（Trifluoromethyl）-1-（propioloyl）-（E）-3-oxo-（2-thienyl）-（2-naphthylamine）

1INTRODUCTIONTheSchiffbasesderivedfromb-diketonesandaliphaticamineshavebeenshowntoexistastheketo-amines.However,ifsubstituentseitherattheketooraminogrouparearomatic,itmaybeexpectedtheenoliminewillbethefavoredtautomericform[1].Recently,someSchiffbasesderivedfromTTA(4,4,4-trifluoro-1-(2-thienyl)-1,3-butanedione)andPMBPhavebeenstudiedbyWang[2]andYu[3]etal.Inordertostudytherelationshipbetweenthestructuresandperformancesofthesecompounds,thetitlecom-poundwillbereportedherein.2EXPERIMENT…     

An Efficient Synthesis of Optically Pure (R)- and (S)-2-(aminomethyl)alanine ((R)- and (S)-ama) and (R)- and (S)-2-(aminomethyl)leucine ((R)- and (S)-aml)

An efficient synthesis of enantiomerically pure (R)- and (S)-2-(aminomethyl)alanine ((R)- and (S)-Ama) 1a and (R)- and (S)-2-(aminomethyl)leucine ((R)- and (S)-Aml) 1b is described (Schemes 1 and 2). Resolution of the racemic amino acids was achieved using L -phenylalanine cyclohexylamide ( 2 ) as chiral auxiliary. The free amino acids 1a, b were converted to the N^α-Boc,N^γ-Z-protected derivatives 11a, b (Scheme 3) ready for incorporation into peptides. Based on the three crystal structures of the diastereoisomeric peptides 8a, 8b , and 9b , the absolute configurations in both series were determined. β-Turn type-I geometries were observed for structures 8b and 9b , whereas 8a crystallized in an extended backbone conformation.     

Syntheses and Structural Characterization of 1-（4-Phenyl-2-thiazolyl）-3-（4-methylphenyl）-5-（2-furyl）-4,5-dihydro-（1H）-pyrazole and 1-（4-（4-Fluoro）phenyl-2-thiazolyl）-3-（4-methyl-phenyl）-5-（2-furyl）-4,5-dihydro-（1H）-pyrazole

The title compounds were synthesized and characterized by IR,1H-NMR,Mass and elementary analysis and single-crystal X-ray diffraction.In 1a,intermolecular C-H…π interactions produce a three-dimensional network.In 1b,intermolecular C-H…O hydrogen bonds generate an R22(22) ring.The hydrogen bonding is supported by C-H…π interactions.     

Smectic A and smectic C materials: partially deuteriated chiral liquid crystals (S)-(-)-2-methylbuty 4-(4-(d13)-hexyloxyphenyl)benzoate and (S)-(-)-2-methylbutyl 4-(4-(d17)-octyloxyphenyl)benzoate

In order to study the difference in microscopic orientation of ferro- and antiferroelectric liquid crystalline molecules, we synthesized the partially deuteriated chiral compounds, (S)-(^-)-2-methylbutyl 4-(4-(d₁₃)-hexyloxy- and (S)-(^-)-2-methylbutyl 4-(4-(d₁₇)-octyloxy-phenyl)benzoates. Fundamental physical properties such as phase transition temperatures, spontaneous polarization and tilt angle were determined. Polarized FTIR measurements were also made to provide information on molecular structure and orientation.     

1-(Triorganylsilyl)-2-(triethoxysilyl)ethanes

Conclusions The conditions were found for the hydrosilylation of CH₂=CHSi(OC₂H₅)₃ with triorganylsilanes in the presence of H₂PtCl₆ · 6H₂O in isopropanol, which assured a high yield (>90%) of the 1-(triorganylsilyl)-2-(tri-ethoxysilyl)ethanes. These conditions were used to synthesize 27 new 1-(triorganylsilyl)-2-(triethoxysilyl)-ethanes.The addition of (C₂H₅O)₃SiH to (CH₂=CHSi(CH₃)₃ in the presence of the same catalyst gave 1-(trimethyl-silyl)-2-(triethoxysilyl)ethane in 98.6% yield.Translated from Izvestiya Akademii Nauk SSSR, Seriya Khimicheskaya, No. 7, pp. 1622–1625, July, 1976.     

Smectic A and smectic C materials: partially deuteriated chiral liquid crystals (S)-(-)-2-methylbuty 4-(4-(d13)-hexyloxyphenyl)benzoate and (S)-(-)-2-methylbutyl 4-(4-(d17)-octyloxyphenyl)benzoate

In order to study the difference in microscopic orientation of ferro- and antiferroelectric liquid crystalline molecules, we synthesized the partially deuteriated chiral compounds, (S)-(^-)-2-methylbutyl 4-(4-(d₁₃)-hexyloxy- and (S)-(^-)-2-methylbutyl 4-(4-(d₁₇)-octyloxy-phenyl)benzoates. Fundamental physical properties such as phase transition temperatures, spontaneous polarization and tilt angle were determined. Polarized FTIR measurements were also made to provide information on molecular structure and orientation.