以偶氮二异庚腈为引发剂的丙烯腈的低温溶液共聚合

以偶氮二异庚腈为引发剂, 丙烯腈、衣康酸和丙烯酸甲酯为三元共聚体系, 在二甲基亚砜中进行低温溶液共聚合, 合成了高分子量的聚丙烯腈树脂. 通过正交设计的方法研究了反应温度、单体浓度和引发剂浓度等因素对分子量和单体转化率的影响, 得出了相应的最佳工艺配方. 采用红外光谱、核磁共振和凝胶渗透色谱等方法对共聚物进行了表征. 结果表明, 降低聚合反应温度和引发剂的用量以及提高单体浓度均有利于提高共聚物的分子量, 其中引发剂浓度对分子量的影响最为显著.     

2,2-diphenyl-1-(trifluoromethanesulphonyl)-hydrazyl

2,2-diphenyl-1-(trifluoromethanesulphonyl)-hydrazyl was prepared by oxidation of the corresponding hydrazine, and is stable in solution. Its ESR spectrum is interpreted in terms of a larger coupling constant for the tricoordinated than for the dicoordinated nitrogen, and of proton coupling constants indicating non-equivalent phenyl groups.     

Synthesis of Dialkyl 1-Methyl-2,2-dichlorocyclopropylcarbonylphosphonates and Alkyl (1-Methyl-2,2-dichlorocyclopropylcarbonyl)arylphosphinates

Russian Journal of General Chemistry -     

Synthesis of 1-morpholino-1-(phenylethynyl)cycloalkanes from enamines and phenylacetylene in the presence of Cu(I) halides

1-Morpholino-1-(phenylethynyl)cyclopentane and 1-morpholino-1-(phenylethynyl)cyclohexane were obtained by reactions of enamines, derivatives of cyclic ketones, with phenylacetylene in the presence of CuI. A scheme for catalysis by Cu(I) compounds with the intermediate formation of copper phenylacetylide and iminium salts was suggested.Translated fromIzvestiya Akademii Nauk. Seriya Khimicheskaya, No. 1, pp. 169–170, January, 1994.     

Synthesis of 3-(4-bromophenyl)-1-morpholino-2-phenylalkan-3-ol hydrochlorides

Reactions of 1-(4-bromophenyl)-3-morpholino-2-phenylpropan-1-one with various Grignard compounds in diethyl ether gave a broad series of tertiary amino alcohols, 3-(4-bromophenyl)-1-morpholino-2-phenylalkan-3-ol hydrochlorides, that can be regarded as Trihexyphenidyl analogs.     

Reaction of 2-methyl-3-morpholino-1-phenylprop-2-en-1-one with Ru3(CO)12

The reaction of Ru₃(CO)₁₂ with 2-methyl-3-morpholino-1-phenylprop-2-en-1-one (1) produced the Ru₆(CO)₁₆(μ₄-η¹:η¹:η²:η²-PhC(O)-C(Me)=C)₂ (2), Ru₂O₂(CO)₄(η³-OC(Ph)C(Me)C(H)C(Me)₂C(Ph))₂ (3), and [Ru(CO)₂(PhCO₂)(O(CH₂-CH₂)₂NH]₂ (4) complexes, which were characterized by IR and NMR spectroscopy. The structures of the complexes were established by X-ray diffraction. The formation of the complexes is accompanied by deamination of ligand 1. Complexes 2 and 3 bearing the vinyl ketone groups contain five-membered oxaruthenacycles and dihydropyran rings. Morpholine is not removed from the reaction mixture and leads to the formation of complex 4. Published in Russian in Izvestiya Akademii Nauk. Seriya Khimicheskaya, No. 12, pp. 2063–2068, December, 2006.     

Synthesis,Crystal Structure and Biological Activity of 1-(3-Amino-4-morpholino-1H-indazole-1-carbonyl)-N-(4-fluorophenyl)cyclopropane-1-carboxamide

The title compound 1-(3-amino-4-morpholino-1 H-indazole-1-carbonyl)-N-(4-fluorophenyl)cyclopropane-1-carboxamide was synthesized by the condensation of 1-[(4-fluorophenyl)carbamoyl]cyclopropane-1-carboxylic acid with 4-morpholino-1 H-indazol-3-amine. This intermediate was prepared from 2,6-difluorobenzonitrile by the condensation with morpholine and then cyclisation with hydrazine hydrate. The crystal structure of the title compound was determined to be of monoclinic system, space group P21/c with a = 10.4645(13), b = 17.368(2), c = 13.7220(13) ? and β = 21.446(7)°. In addition, the compound possesses distinct effective inhibition on the proliferation of HT-29, MKN-45, K562 and A549 cell lines.     

Optically active 1-Alkoxy-2,2-bis(trifluoromethyl)aziridines

1-Alkoxy-2,2-bis(trifluoromethyl)aziridines containing an ester group in the position of the alkoxy substituent undergo nucleophilic substitution (ammonolysis and hydrolysis) with retention of the aziridine ring. The corresponding carboxylic acids, which were separated to give the antipodes with an optical purity of 95% through the diastereomeric salts with R- and S--phenylethylamine, were obtained.Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 11, pp. 1495–1500, November, 1980.     

Hexahydroxybenzene–2,2′-bipyridine (1/2)

2,2′-Bi­pyridine (2BPY) and hexa­hydroxy­benzene (HHB) crystallize in a 2:1 ratio as a neutral molecular adduct, C₆H₆O₆·2C₁₀H₈N₂, in space group P with Z = 1 and with the HHB molecule lying on an inversion centre. HHB, of which this is the first single-crystal X-ray structure determination, forms O—H⃛O hydrogen-bonded chains parallel to the a axis, with O⃛O distances of 2.761 (1) and 2.782 (1) Å. O—H⃛N hydrogen bonds to the 2BPY molecules crosslink these chains, with O⃛N distances of 2.707 (1) and 2.735 (1) Å.     

Synthesis and Crystal Structure of 1-Methylsulfinyl-1-methylthio-2-cyano-2-phenylethylene

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