Two new a-aminophosphonate derivatives containing thieno[2,3-d]pyrimidine, diethyl（（（6-ethyl-2-methyl-4-oxothieno[2,3-d]pyrimidin-3 （4H）-yl）amino）（4-methoxyphenyl）methyl） phosphonate （1） and diethyl（（4-b...Two new a-aminophosphonate derivatives containing thieno[2,3-d]pyrimidine, diethyl（（（6-ethyl-2-methyl-4-oxothieno[2,3-d]pyrimidin-3 （4H）-yl）amino）（4-methoxyphenyl）methyl） phosphonate （1） and diethyl（（4-bromophenyl）（（6-ethyl-2-methyl-4-oxothieno[2,3-d]pyrimidin-3 （4//）-yl）amino）methyl）phosphonate （2）, have been synthesized by a facial phosphorylated reaction, and their structures were characterized by NMR, IR, HRMS and X-ray single-crystal diffraction. Compound 1 （C21H28N3O5PS, Mr = 465.49） belongs to the orthorhombic system, space group P212121, with a = 10.83653（16）, b = 12.04906（19）, c = 18.0061（3） A, V= 2351.06（6） A3, Z= 4, Dc= 1.315 g/cm3, p = 2.177 mm-1, F（000） = 984.0, the final R = 0.0389 and wR = 0.0985 for all data. Compound 2 （C20H25BrN304PS, Mr = 514.37） belongs to the orthorhombic system, space group P212121, with a = 10.9187（5）, b = 11.9522（4）, c = 17.7667（7） A, V= 2318.60（16） A3, Z = 4, Dc= 1.474 g/cm3,μ = 4.175 mm^-1, F（000） = 1056.0, the final R = 0.0367 and wR = 0.0946 for all data.展开更多
The positive and negative ESI-MS/MS spectra of N-ethoxy（phenyl） phosphoryl amino acids（EPP-AA） were investigated by electrospray ionization（ESI） ion trap mass spectrometry. The fragmentation pathways of [ M ＋ N...The positive and negative ESI-MS/MS spectra of N-ethoxy（phenyl） phosphoryl amino acids（EPP-AA） were investigated by electrospray ionization（ESI） ion trap mass spectrometry. The fragmentation pathways of [ M ＋ Na]^＋ and [ M - H]^- ions are proposed and rationalized. The observation may have some potential applications in the interpretation of the MS/MS spectra of novel N-phosphoryl compounds. The complexity of MS/MS spectra of EPP-AA [ M ＋ Na]^＋ ions is decreased compared with that of N-dialkyloxyphosphoryl amino acid. Therefore, the new phosphonamidate method may be considered one of the superior methods that can be used in sequencing peptides and proteins extensively.展开更多
基金supported by the National Natural Science Foundation of China(Nos.21105091 and 21171149)
文摘Two new a-aminophosphonate derivatives containing thieno[2,3-d]pyrimidine, diethyl（（（6-ethyl-2-methyl-4-oxothieno[2,3-d]pyrimidin-3 （4H）-yl）amino）（4-methoxyphenyl）methyl） phosphonate （1） and diethyl（（4-bromophenyl）（（6-ethyl-2-methyl-4-oxothieno[2,3-d]pyrimidin-3 （4//）-yl）amino）methyl）phosphonate （2）, have been synthesized by a facial phosphorylated reaction, and their structures were characterized by NMR, IR, HRMS and X-ray single-crystal diffraction. Compound 1 （C21H28N3O5PS, Mr = 465.49） belongs to the orthorhombic system, space group P212121, with a = 10.83653（16）, b = 12.04906（19）, c = 18.0061（3） A, V= 2351.06（6） A3, Z= 4, Dc= 1.315 g/cm3, p = 2.177 mm-1, F（000） = 984.0, the final R = 0.0389 and wR = 0.0985 for all data. Compound 2 （C20H25BrN304PS, Mr = 514.37） belongs to the orthorhombic system, space group P212121, with a = 10.9187（5）, b = 11.9522（4）, c = 17.7667（7） A, V= 2318.60（16） A3, Z = 4, Dc= 1.474 g/cm3,μ = 4.175 mm^-1, F（000） = 1056.0, the final R = 0.0367 and wR = 0.0946 for all data.
基金Supported by the Education Department of Henan Province(No. 200510459015).
文摘The positive and negative ESI-MS/MS spectra of N-ethoxy（phenyl） phosphoryl amino acids（EPP-AA） were investigated by electrospray ionization（ESI） ion trap mass spectrometry. The fragmentation pathways of [ M ＋ Na]^＋ and [ M - H]^- ions are proposed and rationalized. The observation may have some potential applications in the interpretation of the MS/MS spectra of novel N-phosphoryl compounds. The complexity of MS/MS spectra of EPP-AA [ M ＋ Na]^＋ ions is decreased compared with that of N-dialkyloxyphosphoryl amino acid. Therefore, the new phosphonamidate method may be considered one of the superior methods that can be used in sequencing peptides and proteins extensively.
