As a kind of substrate competition type 5α reductase inhibitor,finasteride is a promising medicine used in the clinical treatment of benign prostatic hyperplasia (BPH).In this paper,a new route for the synthesis of...As a kind of substrate competition type 5α reductase inhibitor,finasteride is a promising medicine used in the clinical treatment of benign prostatic hyperplasia (BPH).In this paper,a new route for the synthesis of finasteride from pregnenolone was proposed.Thus,pregnenolone was converted to finasteride in 10 steps,i.e.,ammoniumation,methoxylation,Oppenauer oxidation,hydrolyzation,cleavage of Δ 4 double bond by oxidation,ring closure by ammonia,hydrogenation of Δ 5 double bond,esterification with methanol,dehydrogenation of 1,2 position in A ring and Bodroux reaction.In this route,expensive reagent 2,2 dipyridyl disulfide commonly used in previous literature was avoided.All of the desired compounds were characterized by MS or/and NMR.The overall yield of finasteride was 13.67% based on pregnenolone.展开更多
The diester diacetylene macrocyclic cyclopentadienone 8 was prepared from the open chain diester acetylene cyclopentadienone 6 in high yield, using the classical Eglinton-Galbraith procedure [1]. Copper(lI) acetate ...The diester diacetylene macrocyclic cyclopentadienone 8 was prepared from the open chain diester acetylene cyclopentadienone 6 in high yield, using the classical Eglinton-Galbraith procedure [1]. Copper(lI) acetate in pyridine was used to effect intramolecular oxidative coupling of 6 under high dilution conditions. During the course of this work a few Diels-Alder reactions of cyclopentadienone 6 were also examined.展开更多
Silver nanoparticles with different morphologies were prepared in AgNO3 aqueous solution using nanocarbon as template medium and polymer surfactant as protecting agent in an ultrasonic field.The polymer surfactant pol...Silver nanoparticles with different morphologies were prepared in AgNO3 aqueous solution using nanocarbon as template medium and polymer surfactant as protecting agent in an ultrasonic field.The polymer surfactant polyvinylpyrrolidone(PVP)was self-prepared and used directly in aqueous solution form.The molecular weight of PVP was measured by viscosimeter.The crystalline phase,component,size,and morphology of the as-synthesized silver naoparticles were characterized by XRD,TEM,FTIR,and Laser Granularity Instrument.The results indicated that ultrasonic was the key factor to deoxidize Ag+ to be Ago,nanocarbon and polymer surfactants accelerated the deoxidization reaction course and controlled the agglomeration of freshly formed silver nanoparticles,the category of polymer surfactant had decisive effect on the morphology of as-synthesized nanoparticle.Well-defined dendrites silver nanoparticle could be attained when choosing PVP as surfactant in AgNO3 aqueous solution,while regular sphere silver nanoparticle could be synthesized in the presence of polyvinyl alcohol(PVA)surfactant.Moreover,the concentration of AgNO3 and ultrasonic action time also had obvious effect on the morphology of silver nanoparticle,low concentration of AgNO3 and long time of ultrasonic were not in favor of forming dendrite silver.展开更多
A novel surface active monomer (surfmer) containing poly(ethylene glycol) chain and terminated phosphate group was synthesized. The copolymerization of synthesized surfmer with NVP (N-vinylpyrrolidone) and with ...A novel surface active monomer (surfmer) containing poly(ethylene glycol) chain and terminated phosphate group was synthesized. The copolymerization of synthesized surfmer with NVP (N-vinylpyrrolidone) and with NVP and VEP (5-tert-butylperoxy-5-methyl-2-hexene-3-yne monomer) led to formation of corresponding surface-active copolymers. The capability of application of resulted copolymers as surface active macroinitiators of emulsion polymerization of styrene and as components of polymeric scaffolds was investigated.展开更多
The flower-like microsphere Bi2WO6 with an average diameter of 2.5 μm is synthesized by a simple hydrothermal method in the presence of surfactant sodium dodecyl sulfate (SDS) or polyvinylpyrrolidone (PVP). The c...The flower-like microsphere Bi2WO6 with an average diameter of 2.5 μm is synthesized by a simple hydrothermal method in the presence of surfactant sodium dodecyl sulfate (SDS) or polyvinylpyrrolidone (PVP). The crystalline phase, compositions, morphology, microstructure, surface area and band gap energy of the Bi2WO6 are characterized by X-ray diffraction, X-ray energy-dispersive spectrum, scanning electron microscopy, transmission electron microscopy and absorption spectra. It is found that surfactant has a significant influence on the microstructure and properties of the samples. The surfaetant SDS en- hances the surface area and photocatalytic activity of Bi2WO6, while the surfactant PVP has an opposite effect. Under Xe lamp irradiation, the Bi2WO6 sample prepared in the presence of SDS can degrade dye Rhodamine B (RhB) effectively.展开更多
A novel silica-supported resin with a cyclic monoamide of polymerized 4-acryloylmorpholine(Silica-AM) was synthesized, and adsorptivity to metal ions of major fission products(FP) was examined in HNO3 and HCl solution...A novel silica-supported resin with a cyclic monoamide of polymerized 4-acryloylmorpholine(Silica-AM) was synthesized, and adsorptivity to metal ions of major fission products(FP) was examined in HNO3 and HCl solutions. Silica-AM has a carbonyl oxygen atom outside of the 6-membered morpholine ring, and a cyclic structure that is different than other cyclic monoamide resins we have studied. These include polyvinylpolypyrrolidone(PVPP) and poly-N-vinyl-ε-caprolactam(VEC), both of which have coordinative carbonyl groups included in the ring. Silica-AM was similar to a cyclic monoamide we have reported because it exhibited adsorption to Pd(Ⅱ) and Re(VⅡ) in HNO3 of a particularly low concentration range. Silica-AM has an ether oxygen atom included in the ring as well. Considering the difference in the chemical structures of Silica-AM and other cyclic monoamide resins, it was suggested that oxygen atoms in the carbonyl group and in ether may be main contributors to Silica-AM's respective adsorptions to Pd(Ⅱ) and Re(VⅡ), and Mo(VI) and Zr(IV). Our results imply that the contribution of the two types of oxygen atoms to adsorption is more observable in an HCl system. The contribution of the ether oxygen atom to the adsorption of Pd(Ⅱ) was also suggested from our study on crystal prepared from 4-acetylmorpholine and palladium nitrate.展开更多
文摘As a kind of substrate competition type 5α reductase inhibitor,finasteride is a promising medicine used in the clinical treatment of benign prostatic hyperplasia (BPH).In this paper,a new route for the synthesis of finasteride from pregnenolone was proposed.Thus,pregnenolone was converted to finasteride in 10 steps,i.e.,ammoniumation,methoxylation,Oppenauer oxidation,hydrolyzation,cleavage of Δ 4 double bond by oxidation,ring closure by ammonia,hydrogenation of Δ 5 double bond,esterification with methanol,dehydrogenation of 1,2 position in A ring and Bodroux reaction.In this route,expensive reagent 2,2 dipyridyl disulfide commonly used in previous literature was avoided.All of the desired compounds were characterized by MS or/and NMR.The overall yield of finasteride was 13.67% based on pregnenolone.
文摘The diester diacetylene macrocyclic cyclopentadienone 8 was prepared from the open chain diester acetylene cyclopentadienone 6 in high yield, using the classical Eglinton-Galbraith procedure [1]. Copper(lI) acetate in pyridine was used to effect intramolecular oxidative coupling of 6 under high dilution conditions. During the course of this work a few Diels-Alder reactions of cyclopentadienone 6 were also examined.
文摘Silver nanoparticles with different morphologies were prepared in AgNO3 aqueous solution using nanocarbon as template medium and polymer surfactant as protecting agent in an ultrasonic field.The polymer surfactant polyvinylpyrrolidone(PVP)was self-prepared and used directly in aqueous solution form.The molecular weight of PVP was measured by viscosimeter.The crystalline phase,component,size,and morphology of the as-synthesized silver naoparticles were characterized by XRD,TEM,FTIR,and Laser Granularity Instrument.The results indicated that ultrasonic was the key factor to deoxidize Ag+ to be Ago,nanocarbon and polymer surfactants accelerated the deoxidization reaction course and controlled the agglomeration of freshly formed silver nanoparticles,the category of polymer surfactant had decisive effect on the morphology of as-synthesized nanoparticle.Well-defined dendrites silver nanoparticle could be attained when choosing PVP as surfactant in AgNO3 aqueous solution,while regular sphere silver nanoparticle could be synthesized in the presence of polyvinyl alcohol(PVA)surfactant.Moreover,the concentration of AgNO3 and ultrasonic action time also had obvious effect on the morphology of silver nanoparticle,low concentration of AgNO3 and long time of ultrasonic were not in favor of forming dendrite silver.
文摘A novel surface active monomer (surfmer) containing poly(ethylene glycol) chain and terminated phosphate group was synthesized. The copolymerization of synthesized surfmer with NVP (N-vinylpyrrolidone) and with NVP and VEP (5-tert-butylperoxy-5-methyl-2-hexene-3-yne monomer) led to formation of corresponding surface-active copolymers. The capability of application of resulted copolymers as surface active macroinitiators of emulsion polymerization of styrene and as components of polymeric scaffolds was investigated.
基金supported by the National High Technology Research and Development Program of China (2009AA03Z217)the National Natural Science Foundation of China (90922028, 50842027)
文摘The flower-like microsphere Bi2WO6 with an average diameter of 2.5 μm is synthesized by a simple hydrothermal method in the presence of surfactant sodium dodecyl sulfate (SDS) or polyvinylpyrrolidone (PVP). The crystalline phase, compositions, morphology, microstructure, surface area and band gap energy of the Bi2WO6 are characterized by X-ray diffraction, X-ray energy-dispersive spectrum, scanning electron microscopy, transmission electron microscopy and absorption spectra. It is found that surfactant has a significant influence on the microstructure and properties of the samples. The surfaetant SDS en- hances the surface area and photocatalytic activity of Bi2WO6, while the surfactant PVP has an opposite effect. Under Xe lamp irradiation, the Bi2WO6 sample prepared in the presence of SDS can degrade dye Rhodamine B (RhB) effectively.
文摘A novel silica-supported resin with a cyclic monoamide of polymerized 4-acryloylmorpholine(Silica-AM) was synthesized, and adsorptivity to metal ions of major fission products(FP) was examined in HNO3 and HCl solutions. Silica-AM has a carbonyl oxygen atom outside of the 6-membered morpholine ring, and a cyclic structure that is different than other cyclic monoamide resins we have studied. These include polyvinylpolypyrrolidone(PVPP) and poly-N-vinyl-ε-caprolactam(VEC), both of which have coordinative carbonyl groups included in the ring. Silica-AM was similar to a cyclic monoamide we have reported because it exhibited adsorption to Pd(Ⅱ) and Re(VⅡ) in HNO3 of a particularly low concentration range. Silica-AM has an ether oxygen atom included in the ring as well. Considering the difference in the chemical structures of Silica-AM and other cyclic monoamide resins, it was suggested that oxygen atoms in the carbonyl group and in ether may be main contributors to Silica-AM's respective adsorptions to Pd(Ⅱ) and Re(VⅡ), and Mo(VI) and Zr(IV). Our results imply that the contribution of the two types of oxygen atoms to adsorption is more observable in an HCl system. The contribution of the ether oxygen atom to the adsorption of Pd(Ⅱ) was also suggested from our study on crystal prepared from 4-acetylmorpholine and palladium nitrate.