A practical synthesis of the 13C/15N-labelled tripeptide N-formyl-Met-Leu-Phe, useful as a reference in solid-state NMR spectroscopy
نویسندگان
چکیده
A mild synthetic method for N-formyl-Met-Leu-Phe-OH (1) is described. After Fmoc solid phase peptide synthesis, on-bead formylation and HPLC purification, more than 30 mg of the fully (13)C/(15)N-labelled tripeptide 1 could be isolated in a typical batch. This peptide can be easily crystallised and is therefore well suited as a standard sample for setting up solid-state NMR experiments.
منابع مشابه
Solid state NMR of isotope labelled murine fur: a powerful tool to study atomic level keratin structure and treatment effects
We have prepared mouse fur extensively 13C,15N-labelled in all amino acid types enabling application of 2D solid state NMR techniques which establish covalent and spatial proximities within, and in favorable cases between, residues. 13C double quantum-single quantum correlation and proton driven spin diffusion techniques are particularly useful for resolving certain amino acid types. Unlike 1D ...
متن کاملSensitivity enhancement in solid-state (13)C NMR of synthetic polymers and biopolymers by (1)H NMR detection with high-speed magic angle spinning.
Indirect detection of 13C and 15N nuclear magnetic resonance (NMR) spectra through 1H NMR signals offers large sensitivity advantages in studies of organic and biological molecules in solution and is almost universally employed.1-3 Although sensitivity enhancement by indirect detection was first demonstrated in NMR4-6 and nuclear quadrupole resonance7,8 of solids, direct detection has generally...
متن کاملDetermination of multiple torsion-angle constraints in U-(13)C,(15)N-labeled peptides: 3D (1)H-(15)N-(13)C-(1)H dipolar chemical shift NMR spectroscopy in rotating solids.
We demonstrate constraint of peptide backbone and side-chain conformation with 3D (1)H-(15)N-(13)C-(1)H dipolar chemical shift, magic-angle spinning NMR experiments. In these experiments, polarization is transferred from (15)N[i] by ramped SPECIFIC cross polarization to the (13)C(alpha)[i], (13)C(beta)[i], and (13)C(alpha)[i - 1] resonances and evolves coherently under the correlated (1)H-(15)N...
متن کاملThe Use of 13C in the Synthesis of Double Labelled Precursors
Discovery of 13C NMR and its application in the biosynthetic pathways prompted the synthesis of several 13C labelled precursors. To investigate the metabolism of phenyllactic acid in the Solanaceae family, the double labelled acid was synthesized from barium carbonate (13C) and sodium syanide (13C)
متن کاملSolid state synthesis of NiO nanoparticles from [(1,2-bis(2-formyl-3-methoxyphenyl)propane)nickel(II)] chloride
In this paper, nickel oxide (NiO) nanoparticles have been prepared by solid state thermal decomposition of an acyclic nickel(II) complex (1,2-bis(2-formyl-3-methoxyphenyl)propane)nickel(II) chloride, [NiL]Cl2, in an electrical furnace at optimal temperature, 450 ºC for 3.5 h. The nickel(II) complex is obtained via solid state synthesis using nickel(II) chloride and tetradentate O4 acyclic ligan...
متن کاملذخیره در منابع من
با ذخیره ی این منبع در منابع من، دسترسی به آن را برای استفاده های بعدی آسان تر کنید
برای دانلود متن کامل این مقاله و بیش از 32 میلیون مقاله دیگر ابتدا ثبت نام کنید
ثبت ناماگر عضو سایت هستید لطفا وارد حساب کاربری خود شوید
ورودعنوان ژورنال:
- Beilstein Journal of Organic Chemistry
دوره 4 شماره
صفحات -
تاریخ انتشار 2008