Capillary electrophoresis coupled to mass spectrometry（CE–MS） was used for the analysis of naphthenic acid fraction compounds（NAFCs） of oil sands process-affected water（OSPW）. A standard mixture of amine-deriva...Capillary electrophoresis coupled to mass spectrometry（CE–MS） was used for the analysis of naphthenic acid fraction compounds（NAFCs） of oil sands process-affected water（OSPW）. A standard mixture of amine-derivatized naphthenic acids is injected directly onto the CE column and analyzed by CE–MS in less than 15 min. Time of flight MS analysis（TOFMS）, optimized for high molecular weight ions, showed NAFCs between 250 and 800 m/z. With a quadrupole mass analyzer, only low-molecular weight NAFCs（between 100 and 450 m/z） are visible under our experimental conditions. Derivatization of NAFCs consisted of two-step amidation reactions mediated by 1-ethyl-3-（3-dimethylaminopropyl）carbodiimide（EDC）, or mediated by a mixture of EDC and N-hydroxysuccinimide, in dimethyl sulfoxide, dichloromethane or ethyl acetate. The optimum background electrolyte composition was determined to be 30%（V/V） methanol in water and 2%（V/V） formic acid. NAFCs extracted from OSPW in the Athabasca oil sands region were used to demonstrate the feasibility of CE–MS for the analysis of NAFCs in environmental samples, showing that the labeled naphthenic acids are in the mass range of 350 to 1500 m/z.展开更多
4（3H）-Quinazolinones have been synthesized from poly（ethylene glycol） （PEG） supported aza-Wittig reaction. 2-Dialkylamino- 4（3H）-quinazolinones 6 were synthesized efficiently by reaction of secondary amine wit...4（3H）-Quinazolinones have been synthesized from poly（ethylene glycol） （PEG） supported aza-Wittig reaction. 2-Dialkylamino- 4（3H）-quinazolinones 6 were synthesized efficiently by reaction of secondary amine with PEG-supported carbodiimides 4, which were obtained from aza-Wittig reaction of PEG-supported iminophosphoranes 3 with isocyanates.展开更多
The title compounds 3,5,6,7-tetrahydro-4H-cyclopenta[4,5]thieno[2,3-d]pyrimidin-4-ones（6） were synthesized by base catalytic reactions of secondary amines with carbodiimides 4, which were obtained from the aza-Witti...The title compounds 3,5,6,7-tetrahydro-4H-cyclopenta[4,5]thieno[2,3-d]pyrimidin-4-ones（6） were synthesized by base catalytic reactions of secondary amines with carbodiimides 4, which were obtained from the aza-Wittig reaction of iminophosphoranes（3） with aromatic isocyanates.展开更多
基金supported by the Environment Canada and the NSERC
文摘Capillary electrophoresis coupled to mass spectrometry（CE–MS） was used for the analysis of naphthenic acid fraction compounds（NAFCs） of oil sands process-affected water（OSPW）. A standard mixture of amine-derivatized naphthenic acids is injected directly onto the CE column and analyzed by CE–MS in less than 15 min. Time of flight MS analysis（TOFMS）, optimized for high molecular weight ions, showed NAFCs between 250 and 800 m/z. With a quadrupole mass analyzer, only low-molecular weight NAFCs（between 100 and 450 m/z） are visible under our experimental conditions. Derivatization of NAFCs consisted of two-step amidation reactions mediated by 1-ethyl-3-（3-dimethylaminopropyl）carbodiimide（EDC）, or mediated by a mixture of EDC and N-hydroxysuccinimide, in dimethyl sulfoxide, dichloromethane or ethyl acetate. The optimum background electrolyte composition was determined to be 30%（V/V） methanol in water and 2%（V/V） formic acid. NAFCs extracted from OSPW in the Athabasca oil sands region were used to demonstrate the feasibility of CE–MS for the analysis of NAFCs in environmental samples, showing that the labeled naphthenic acids are in the mass range of 350 to 1500 m/z.
基金We gratefully acknowledge financial support of this work by the Natural Science Foundation of Hubei Province （No. 2006ABB016） the National Natural Science Foundation of China （No. 20772041） Key Project of Chinese Ministry of Education （No. 107082）.
文摘4（3H）-Quinazolinones have been synthesized from poly（ethylene glycol） （PEG） supported aza-Wittig reaction. 2-Dialkylamino- 4（3H）-quinazolinones 6 were synthesized efficiently by reaction of secondary amine with PEG-supported carbodiimides 4, which were obtained from aza-Wittig reaction of PEG-supported iminophosphoranes 3 with isocyanates.
基金the National Natural Science Foundation of China(No.20772041)the Opening Foundation of the Key Labo-ratory of Three Gorges University of China(No.2006NP01)the Key Project of Chinese Ministry of Education(No.107082)
文摘The title compounds 3,5,6,7-tetrahydro-4H-cyclopenta[4,5]thieno[2,3-d]pyrimidin-4-ones（6） were synthesized by base catalytic reactions of secondary amines with carbodiimides 4, which were obtained from the aza-Wittig reaction of iminophosphoranes（3） with aromatic isocyanates.
