The title compound ethyl 2-（6-（1,3-dioxo-4,5,6,7-tetrahydro-lH-isoindol-2（3H）- yl）-7-fluoro-3-oxo-2H-benzo[b][1,4]oxazin-4（3H）-yl） butanoate 3 was synthesized by the reaction of ethyl 2-（6-amino-7-fluoro-3-ox...The title compound ethyl 2-（6-（1,3-dioxo-4,5,6,7-tetrahydro-lH-isoindol-2（3H）- yl）-7-fluoro-3-oxo-2H-benzo[b][1,4]oxazin-4（3H）-yl） butanoate 3 was synthesized by the reaction of ethyl 2-（6-amino-7-fluoro-3-oxo-2H-benzo[b][1,4]oxazin-4（3H）-yl） butanoate with 4,5,6,7- tetraydrophthalic anhydride, and its structure was determined by X-ray single-crystal diffraction. The crystal belongs to the monoclinic system, space group P2 1/n with a = 9.3469（2）, b = 16.7715（5）, c = 13.7153（4） A, β= 104.9680（10）°, μ = 0.107 mm^-1, Mr = 430.42, V= 2077.08（10） ,A3, Z= 4, Dc = 1.376 g/cm3, F（000） = 904, T= 296（2） K, R = 0.0508 and wR = 0.1478.展开更多
The ring-opening polymerization of 1,4-dioxan-2-one （PDO） was carried out by lanthanum tris（2,6-di-tert-butyl-4- methylphenolate） （La（OAr）3） as novel single component initiaLor. The influences of polymerizatio...The ring-opening polymerization of 1,4-dioxan-2-one （PDO） was carried out by lanthanum tris（2,6-di-tert-butyl-4- methylphenolate） （La（OAr）3） as novel single component initiaLor. The influences of polymerization reaction temperature and the molar ratio of monomer to initiator on the monomer conversion and molecular weight of poly（1,4-dioxan-2-one） （PPDO） were explored. PPDO with high viscosity average molecular weight of 1.95×10^5 can be prepared at 40℃ when [PDO]/ [La（OAr）3] molar ratio was 800. Mechanism investigation shows that the polymerization proceeds through a ＂coordination- insertion＂ mechanism with selective rupture of acyl-oxygen be,nd of PDO.展开更多
Some 2 (2 chloro ethoxy) acetates were prepared by the reaction of 2 oxo 1,4 dixane with alcohol and thionyl chloride.Some reactions of ethyl 2 (2 chloro ethoxy) acetate were studied.2 Oxo 1,4 dixane was obtained rene...Some 2 (2 chloro ethoxy) acetates were prepared by the reaction of 2 oxo 1,4 dixane with alcohol and thionyl chloride.Some reactions of ethyl 2 (2 chloro ethoxy) acetate were studied.2 Oxo 1,4 dixane was obtained renewably by the reaction of ethyl 2 (2 chloro ethoxy) acetate base catalyzed hydrolysis.Under the condition of acid catalyzed hydrolysis,2 (2 chloro ethoxy) acetic acid was obtained.Using IR, 1HNMR and elemental analysis characterized these compounds that mentioned above using MS to confirme some compounds.展开更多
Cultivation of an endophytic fungus Aspergillus niger EN-13 that was isolated from the inner tissue of the marine brown alga Colpomenia sinuosa resulted in the characterization of a new naphthoquinoneimine derivative,...Cultivation of an endophytic fungus Aspergillus niger EN-13 that was isolated from the inner tissue of the marine brown alga Colpomenia sinuosa resulted in the characterization of a new naphthoquinoneimine derivative, namely, 5,7-dihydroxy-2-[1-（4- methoxy-6-oxo-6H-pyran-2-yl）-2-phenylethylamino]-[ 1,4]naphthoquinone. The structure of the new compound was established on the basis of various NMR spectroscopic analyses including 2D NMR techniques, El-MS, and HR-ESI-MS. This compound displayed moderate antifungal activity.展开更多
建立了高效液相色谱法测定雷贝拉唑钠肠溶片中的1-(1H-苯并咪唑-2-基)-3-甲基-4-氧代-1,4-二氢吡啶-2-羧酸钠。采用氨基色谱柱,以0.05 mol/L磷酸二氢钠溶液(用磷酸调至p H 3.0)∶乙腈(60∶40)为流动相,检测波长290 nm。1-(1H-苯并咪唑-2...建立了高效液相色谱法测定雷贝拉唑钠肠溶片中的1-(1H-苯并咪唑-2-基)-3-甲基-4-氧代-1,4-二氢吡啶-2-羧酸钠。采用氨基色谱柱,以0.05 mol/L磷酸二氢钠溶液(用磷酸调至p H 3.0)∶乙腈(60∶40)为流动相,检测波长290 nm。1-(1H-苯并咪唑-2-基)-3-甲基-4-氧代-1,4-二氢吡啶-2-羧酸钠在0.05~20?g/ml浓度范围内线性关系良好,回收率为95.7%,RSD为6.6%。展开更多
New initiator systems for the ring-opening polymerization of 1,4-dioxan-2-one (PDO), AlEt 3-M(AcAc) n-H 2O, where M=Nd, La, Zn, Fe, Co and Ni, were used to initiate the ring-opening polymerization of PDO in bulk, and ...New initiator systems for the ring-opening polymerization of 1,4-dioxan-2-one (PDO), AlEt 3-M(AcAc) n-H 2O, where M=Nd, La, Zn, Fe, Co and Ni, were used to initiate the ring-opening polymerization of PDO in bulk, and to synthesize poly(1,4-dioxan-2-one)(PPDO) with high molecular weights within very short reaction time. A high conversion of monomer can be reached. Of all those initiator systems, AlEt 3-Nd(AcAc) 3-H 2O is the best one. The effects of n(Al)∶n(Nd) and n(H 2O)∶n(Al) on the polymerization of PDO were investigated. It was found that n(AlEt 3)∶ n[Nd(AcAc) 3]∶n(H 2O)=8∶1∶4 could obtain the best initiating effects. PPDO with a viscosity-average molecular weight of 3.1×105 can be obtained when n(PDO)∶n[AlEt 3-Nd(AcAc) 3-H 2O] is 2 000, the reaction temperature 80 ℃, and the reaction time 24 h. Meanwhile, a high conversion of 94.7% can be reached.展开更多
基金Supported by the National Natural Science Foundation of China (20872033, 20575019)Natural Science Foundation of Hunan Province (07JJ1003)+1 种基金Key Laboratory of Chemical Biology and Traditional Chinese Medicine Research (Ministry of Education of China) (KLCBTCMR2008-14)Scientific Research Fund of Science and Technology Department of Hunan Province (No. 2006GK3067)
文摘The title compound ethyl 2-（6-（1,3-dioxo-4,5,6,7-tetrahydro-lH-isoindol-2（3H）- yl）-7-fluoro-3-oxo-2H-benzo[b][1,4]oxazin-4（3H）-yl） butanoate 3 was synthesized by the reaction of ethyl 2-（6-amino-7-fluoro-3-oxo-2H-benzo[b][1,4]oxazin-4（3H）-yl） butanoate with 4,5,6,7- tetraydrophthalic anhydride, and its structure was determined by X-ray single-crystal diffraction. The crystal belongs to the monoclinic system, space group P2 1/n with a = 9.3469（2）, b = 16.7715（5）, c = 13.7153（4） A, β= 104.9680（10）°, μ = 0.107 mm^-1, Mr = 430.42, V= 2077.08（10） ,A3, Z= 4, Dc = 1.376 g/cm3, F（000） = 904, T= 296（2） K, R = 0.0508 and wR = 0.1478.
基金This work was financially supported by the financial support of National Natural Science Foundation of China (No. 20434020)
文摘The ring-opening polymerization of 1,4-dioxan-2-one （PDO） was carried out by lanthanum tris（2,6-di-tert-butyl-4- methylphenolate） （La（OAr）3） as novel single component initiaLor. The influences of polymerization reaction temperature and the molar ratio of monomer to initiator on the monomer conversion and molecular weight of poly（1,4-dioxan-2-one） （PPDO） were explored. PPDO with high viscosity average molecular weight of 1.95×10^5 can be prepared at 40℃ when [PDO]/ [La（OAr）3] molar ratio was 800. Mechanism investigation shows that the polymerization proceeds through a ＂coordination- insertion＂ mechanism with selective rupture of acyl-oxygen be,nd of PDO.
文摘Some 2 (2 chloro ethoxy) acetates were prepared by the reaction of 2 oxo 1,4 dixane with alcohol and thionyl chloride.Some reactions of ethyl 2 (2 chloro ethoxy) acetate were studied.2 Oxo 1,4 dixane was obtained renewably by the reaction of ethyl 2 (2 chloro ethoxy) acetate base catalyzed hydrolysis.Under the condition of acid catalyzed hydrolysis,2 (2 chloro ethoxy) acetic acid was obtained.Using IR, 1HNMR and elemental analysis characterized these compounds that mentioned above using MS to confirme some compounds.
基金partially supported by the fund of Key Laboratory of Marine Drugs(0cean University of China),Ministry of Education[KLMD(0UC)2004]by the National Natural Science Foundation of China(No.30530080)+1 种基金A program supported by the Department of Science and Technology of Shandong Province(No.2006GG2205023)by the Guangdong Key Laboratory of Marine Materia Medica is also gratefully acknowledged.
文摘Cultivation of an endophytic fungus Aspergillus niger EN-13 that was isolated from the inner tissue of the marine brown alga Colpomenia sinuosa resulted in the characterization of a new naphthoquinoneimine derivative, namely, 5,7-dihydroxy-2-[1-（4- methoxy-6-oxo-6H-pyran-2-yl）-2-phenylethylamino]-[ 1,4]naphthoquinone. The structure of the new compound was established on the basis of various NMR spectroscopic analyses including 2D NMR techniques, El-MS, and HR-ESI-MS. This compound displayed moderate antifungal activity.
文摘建立了高效液相色谱法测定雷贝拉唑钠肠溶片中的1-(1H-苯并咪唑-2-基)-3-甲基-4-氧代-1,4-二氢吡啶-2-羧酸钠。采用氨基色谱柱,以0.05 mol/L磷酸二氢钠溶液(用磷酸调至p H 3.0)∶乙腈(60∶40)为流动相,检测波长290 nm。1-(1H-苯并咪唑-2-基)-3-甲基-4-氧代-1,4-二氢吡啶-2-羧酸钠在0.05~20?g/ml浓度范围内线性关系良好,回收率为95.7%,RSD为6.6%。
文摘New initiator systems for the ring-opening polymerization of 1,4-dioxan-2-one (PDO), AlEt 3-M(AcAc) n-H 2O, where M=Nd, La, Zn, Fe, Co and Ni, were used to initiate the ring-opening polymerization of PDO in bulk, and to synthesize poly(1,4-dioxan-2-one)(PPDO) with high molecular weights within very short reaction time. A high conversion of monomer can be reached. Of all those initiator systems, AlEt 3-Nd(AcAc) 3-H 2O is the best one. The effects of n(Al)∶n(Nd) and n(H 2O)∶n(Al) on the polymerization of PDO were investigated. It was found that n(AlEt 3)∶ n[Nd(AcAc) 3]∶n(H 2O)=8∶1∶4 could obtain the best initiating effects. PPDO with a viscosity-average molecular weight of 3.1×105 can be obtained when n(PDO)∶n[AlEt 3-Nd(AcAc) 3-H 2O] is 2 000, the reaction temperature 80 ℃, and the reaction time 24 h. Meanwhile, a high conversion of 94.7% can be reached.
