A new monomer, 1,4-bis(4-fluorobenzoyl) naphthalene(compound 2) was synthesized via a two-step reaction. 1,4-Naphthalenedicarboxylic acid chloride(compound 1) was prepared by using the acyl chlorization reaction of 1,...A new monomer, 1,4-bis(4-fluorobenzoyl) naphthalene(compound 2) was synthesized via a two-step reaction. 1,4-Naphthalenedicarboxylic acid chloride(compound 1) was prepared by using the acyl chlorization reaction of 1,4-naphthalenedicarboxylic acid with thionyl chloride. The Friedel-Crafts acylation of compound 1 with fluorobenzene afforded compound 2 in a 80% yield. The polycondensation of compound 2 with various bisphenols in tetramethylene sulfone(TMS) in the presence of excess potassium carbonate as a condensation reagent was carried out at 210 ℃ to quantitatively afford the corresponding poly(aryl ether ketone)s(compounds 3_8) containing 1,4-naphthalene moieties. Thermal analyses showed that the polymers have T g values ranging from 496 to 500 K and are thermally stable in air with initial mass loss above 500 ℃. These novel polymers exhibited an excellent solubility in organic solvents including NMP, DMAc, and chloroform, etc. In addition, the glass transition temperatures of these polymers increased and the polymers became insoluble in chloroform after treated at 260 ℃, indicating the occurrence of a thermal crosslinking reaction.展开更多
Poly（ aryl ether ketone） copolymers containing 2,7-naphthylene and hydroquinone（HQ） moieties with various compositions were prepared by the reaction of 4,4＇-difluorobenzophenone（DFB） 2,7-naphthylene and hydroqu...Poly（ aryl ether ketone） copolymers containing 2,7-naphthylene and hydroquinone（HQ） moieties with various compositions were prepared by the reaction of 4,4＇-difluorobenzophenone（DFB） 2,7-naphthylene and hydroquinone in the presence of sodium carbonate and potassium carbonate （ 19： 1, mass ratio） in diphenyl sulfone （DPS）. The thermal analysis results of the copolymers show that the glass transition temperatures（Tgs） increase, while the melting temperatures（Tra） and tile 5.0% weight loss temperatures （ Td ） decrease with the increase of the 2,7-naphthalene moieties. For the copolymers synthesized at a molar fraction of 2,7-naphthalene in the difluoro monomers being over 0.30, no peaks corresponding to the cold crystallization temperature and the melting temperature could be detected, indicating that these copolymers are almost amorphous. The crystal structures of the copolymers with a molar fraction of 2,7-naphthalene being less than 0. 30 are rhombic.展开更多
Sodium deoxycholate (NaDOC) could induce 1-bromo-4-(bromoacetyl) naphthalene (BBAN) to emit strong room temperature phosphorescence (RTP). Measurements of phosphore- scence spectra, peak intensity and polarization we...Sodium deoxycholate (NaDOC) could induce 1-bromo-4-(bromoacetyl) naphthalene (BBAN) to emit strong room temperature phosphorescence (RTP). Measurements of phosphore- scence spectra, peak intensity and polarization were used to investigate the solubilization of BBAN as a function of NaDOC concentration.展开更多
Three new naphthaline-type chromophores end-capped with different (p-substituted amino) styryl groups on the both sides (named as BPASN, BHMASN and BMASN) have been synthesized. Under excitation of 380 nm, strong gree...Three new naphthaline-type chromophores end-capped with different (p-substituted amino) styryl groups on the both sides (named as BPASN, BHMASN and BMASN) have been synthesized. Under excitation of 380 nm, strong green light-emitting locating at 517 nm with the fluorescence quantum yield of 0.88 in CH2Cl2 has been obtained. In the presence of b-cyclodextrin (b-CD), strong blue-emitting at 456 nm in DMF was also recorded.展开更多
We substituted several environmentally friendly catalysts which included HY and H- β zeolites, various cation-exchanged β zeolites, and solid-supported ferric chloride for conventional catalysts for the synth...We substituted several environmentally friendly catalysts which included HY and H- β zeolites, various cation-exchanged β zeolites, and solid-supported ferric chloride for conventional catalysts for the synthesis of 3-(1-cyclohexenyl)-2-butanone from the reaction of ethylidenecyclohexane with acetic anhydride at room temperature. HY zeolite was found to be the most effective for this reaction, and gave the acylated product in a 72% yield under the conditions of n (ethylidenecyclohexane)/ n (acetic anhydride)/ m (HY zeolite)=1 mmol/10 mmol/0 100 g, reaction temperature 25 ℃ and reaction time 2 h. The used HY zeolite can be recovered, regenerated and gave almost the same yield as the fresh one. The lifetime of the HY zeolite is over 80 h. The effect of different factors on the reaction has also been investigated.展开更多
A convenient one-pot synthesis of functionalized （E）-2-arylvinyl bromides was achieved by microwave-induced deacetylation and subsequent acylation using dicyclohexyl carbodiimide （DCC） and dimethylamino-pyridine ...A convenient one-pot synthesis of functionalized （E）-2-arylvinyl bromides was achieved by microwave-induced deacetylation and subsequent acylation using dicyclohexyl carbodiimide （DCC） and dimethylamino-pyridine （DMAP） at room temperature from （E）-4-（2-bromovinyl）phenyl acetate.展开更多
A concise and efficient method for the synthesis of novel 9,10-imethoxybenzo[6,7]oxepino[3,4-b]quinolin13(6H)-one and its derivatives 7a-p has been developed via the intramolecular Friedel-Crafts acylation reactions o...A concise and efficient method for the synthesis of novel 9,10-imethoxybenzo[6,7]oxepino[3,4-b]quinolin13(6H)-one and its derivatives 7a-p has been developed via the intramolecular Friedel-Crafts acylation reactions of 6,7-dimethoxy-2-(phenoxymethyl)quinoline-3-carboxylic acids 6a-p with polyphosphoric acid (PPA) as catalyst and solvent under mild conditions. The key intermediates 6a-p were prepared through the in situ formation of ethyl 6,7-dimethoxy-2-(phenoxymethyl)quinoline-3-carboxylates 5a-p followed by hydrolysis with aqueous ethanolic sodium hydroxide solution. The novel synthetic method has the advantages of good yields, easy work-up, and environmentally friendly character, which may provide a novel highly efficient process for making quinoline and related azaheterocycle libraries.展开更多
An oxetane ring can be constructed from 5α-acyloxy-Δ4(20)-taxoids. Hie facile intramolecular acyl migration from 5- to 20-position under slightly basic conditions enabled the construction of the oxetane ring in a co...An oxetane ring can be constructed from 5α-acyloxy-Δ4(20)-taxoids. Hie facile intramolecular acyl migration from 5- to 20-position under slightly basic conditions enabled the construction of the oxetane ring in a convenient short cut, whereas the acyl migration from 2- to 20-position left the 2-hydroxyl accessible to a later benzoylation. An unexpected five-mem-bered 4-O, 20- O sulfite ring was formed in the attempted construction of the oxetane ring with 5α-triflate as a leaving group. After the construction of the oxetane ring, treatment with strong base LiHMDS and acetyl chloride gave the expected 4-O-acetate while treatment with acetic anhydride and DMAP gave a 4-O-acetoacetate.展开更多
基金Supported by the National Natural Science Foundation of China(No.5 0 2 0 30 0 4 )
文摘A new monomer, 1,4-bis(4-fluorobenzoyl) naphthalene(compound 2) was synthesized via a two-step reaction. 1,4-Naphthalenedicarboxylic acid chloride(compound 1) was prepared by using the acyl chlorization reaction of 1,4-naphthalenedicarboxylic acid with thionyl chloride. The Friedel-Crafts acylation of compound 1 with fluorobenzene afforded compound 2 in a 80% yield. The polycondensation of compound 2 with various bisphenols in tetramethylene sulfone(TMS) in the presence of excess potassium carbonate as a condensation reagent was carried out at 210 ℃ to quantitatively afford the corresponding poly(aryl ether ketone)s(compounds 3_8) containing 1,4-naphthalene moieties. Thermal analyses showed that the polymers have T g values ranging from 496 to 500 K and are thermally stable in air with initial mass loss above 500 ℃. These novel polymers exhibited an excellent solubility in organic solvents including NMP, DMAc, and chloroform, etc. In addition, the glass transition temperatures of these polymers increased and the polymers became insoluble in chloroform after treated at 260 ℃, indicating the occurrence of a thermal crosslinking reaction.
文摘Poly（ aryl ether ketone） copolymers containing 2,7-naphthylene and hydroquinone（HQ） moieties with various compositions were prepared by the reaction of 4,4＇-difluorobenzophenone（DFB） 2,7-naphthylene and hydroquinone in the presence of sodium carbonate and potassium carbonate （ 19： 1, mass ratio） in diphenyl sulfone （DPS）. The thermal analysis results of the copolymers show that the glass transition temperatures（Tgs） increase, while the melting temperatures（Tra） and tile 5.0% weight loss temperatures （ Td ） decrease with the increase of the 2,7-naphthalene moieties. For the copolymers synthesized at a molar fraction of 2,7-naphthalene in the difluoro monomers being over 0.30, no peaks corresponding to the cold crystallization temperature and the melting temperature could be detected, indicating that these copolymers are almost amorphous. The crystal structures of the copolymers with a molar fraction of 2,7-naphthalene being less than 0. 30 are rhombic.
文摘Sodium deoxycholate (NaDOC) could induce 1-bromo-4-(bromoacetyl) naphthalene (BBAN) to emit strong room temperature phosphorescence (RTP). Measurements of phosphore- scence spectra, peak intensity and polarization were used to investigate the solubilization of BBAN as a function of NaDOC concentration.
文摘Three new naphthaline-type chromophores end-capped with different (p-substituted amino) styryl groups on the both sides (named as BPASN, BHMASN and BMASN) have been synthesized. Under excitation of 380 nm, strong green light-emitting locating at 517 nm with the fluorescence quantum yield of 0.88 in CH2Cl2 has been obtained. In the presence of b-cyclodextrin (b-CD), strong blue-emitting at 456 nm in DMF was also recorded.
基金Supported by the National Natural Science Foundation of China( No.2 0 1730 14 )
文摘We substituted several environmentally friendly catalysts which included HY and H- β zeolites, various cation-exchanged β zeolites, and solid-supported ferric chloride for conventional catalysts for the synthesis of 3-(1-cyclohexenyl)-2-butanone from the reaction of ethylidenecyclohexane with acetic anhydride at room temperature. HY zeolite was found to be the most effective for this reaction, and gave the acylated product in a 72% yield under the conditions of n (ethylidenecyclohexane)/ n (acetic anhydride)/ m (HY zeolite)=1 mmol/10 mmol/0 100 g, reaction temperature 25 ℃ and reaction time 2 h. The used HY zeolite can be recovered, regenerated and gave almost the same yield as the fresh one. The lifetime of the HY zeolite is over 80 h. The effect of different factors on the reaction has also been investigated.
基金supported by the Natural Science Foundation of Shanghai,China(No.06ZR14085)the Scientific Research Foundation for the Returned Overseas Chinese Scholars,State Education Ministry.
文摘A convenient one-pot synthesis of functionalized （E）-2-arylvinyl bromides was achieved by microwave-induced deacetylation and subsequent acylation using dicyclohexyl carbodiimide （DCC） and dimethylamino-pyridine （DMAP） at room temperature from （E）-4-（2-bromovinyl）phenyl acetate.
文摘A concise and efficient method for the synthesis of novel 9,10-imethoxybenzo[6,7]oxepino[3,4-b]quinolin13(6H)-one and its derivatives 7a-p has been developed via the intramolecular Friedel-Crafts acylation reactions of 6,7-dimethoxy-2-(phenoxymethyl)quinoline-3-carboxylic acids 6a-p with polyphosphoric acid (PPA) as catalyst and solvent under mild conditions. The key intermediates 6a-p were prepared through the in situ formation of ethyl 6,7-dimethoxy-2-(phenoxymethyl)quinoline-3-carboxylates 5a-p followed by hydrolysis with aqueous ethanolic sodium hydroxide solution. The novel synthetic method has the advantages of good yields, easy work-up, and environmentally friendly character, which may provide a novel highly efficient process for making quinoline and related azaheterocycle libraries.
基金Project supported by Chinese Academy of Medical Science Researeh Grant and Taisho Pharmaceutical Co. Ltd.
文摘An oxetane ring can be constructed from 5α-acyloxy-Δ4(20)-taxoids. Hie facile intramolecular acyl migration from 5- to 20-position under slightly basic conditions enabled the construction of the oxetane ring in a convenient short cut, whereas the acyl migration from 2- to 20-position left the 2-hydroxyl accessible to a later benzoylation. An unexpected five-mem-bered 4-O, 20- O sulfite ring was formed in the attempted construction of the oxetane ring with 5α-triflate as a leaving group. After the construction of the oxetane ring, treatment with strong base LiHMDS and acetyl chloride gave the expected 4-O-acetate while treatment with acetic anhydride and DMAP gave a 4-O-acetoacetate.
