Peptides-XXXXVI: Studies in the synthesis of an analogue of hen egg white lysozyme

The previously synthesised (1–37), (38–75), (76–93), (94–104), (105–117) and (118–129) fragments of the analogue were combined making extensive use of the DCCI/HONSu method. The final coupling involved the (1–75) and (76–129) sub-fragments. Aggregation of the latter fragment caused problems in purification by routine gel filtration methods employing Enzacryl K2 or Sephadex LH60. The fully protected (1–129) product was partially purified by washing, then deprotectcd and purified by gel filtration and ion exchange chromatography. Satisfactory removal of the acetamidomethyl group used for cysteine protection could not be achieved.     

Gel filtration of protected peptides on sephadex G-50 in hexamethylphosphoramide containing 5% water.

Gel permeation chromatography on G-50 and G-75 Sephadex gels, using 5% water in hexamethylphosphoramide (phosphoric trisdimethylamide) has been applied to the purification of large protected peptides which are outside the molecular weight range of the Sephadex LH-20-dimethylformamide system.     

Peptides—XXXVII: Synthesis of the 1–37 fragment of a lysozyme analogue

Combination of the protected peptide fragments 1–16, 17–26 and 27–37 to yield the 1–37 portion of a lysozyme analogue is described. The fragments were combined using DCCI with the addition of HONSu, and the products purified mainly by gel filtration.     

Peptides—XXXX: Synthesis of the 68–75 fragment of a lysozyme analogue

The 68–75 subfragment has been prepared by a 4+4 fragment condensation using DCCI/HOBt. The constituent 68–71 and 72–75 fragments being prepared stepwise by the pivalic mixed anhydride method. The octapeptide prepared by this approach was shown to be identical with that synthesised by a solid phase method using a phenolic polymer as the support.     

Peptides—XXXV: Synthesis of the 17–26 fragment of a lysozyme analogue

The fully protected 17–26 fragment of a lysozyme analogue has been synthesised. A fragment condensation approach has been employed using the protected subfragments 17–19, 20–22 and 23–26. In the synthesis of the subfragments the use of the diphenylphosphinyl mixed anhydride method has been demonstrated.     

Measurement of gamow-teller strength for 176Yb --> 176Lu and the efficiency of a solar neutrino detector

We report a 0 degrees 176Yb(p,n)176Lu measurement at IUCF where we used 120 and 160 MeV protons and the energy dependence method to determine Gamow-Teller (GT) matrix elements relative to the model independent Fermi matrix element. The data show that there is an isolated concentration of GT strength in the low-lying 1(+) states making the proposed Low Energy Neutrino Spectroscopy detector (based on neutrino captures on 176Yb) sensitive to pp and 7Be neutrinos and a promising detector to resolve the solar neutrino problem.     

The diffraction of elastic waves by an imperfect fusion bond

We consider diffraction by a semi-infinite crack located alonga fusion interface between two differing elastic media. Twotypes of crack, namely open and partially closed cracks, areinvestigated. An open crack is modelled by a stress-free contactboundary condition and a partially closed crack is modelledby a spring contact boundary condition. For the latter, thejump in the stress across the crack is assumed to be proportionalto the jump in the displacement across the crack. This situationarises in, for example, a K-weld where the fine grain of theparent material (for example, ferritic or forged austeniticsteel) is in stark contrast with the coarse-grained weld metal(for example, austenitic weld metal). In the metal weld thedirection of the grain axis varies through the metal. However,diffraction is a local phenomenon and so the austenitic steelis assumed to have a zonal axis so that it may be modelled bya transversely isotropic composite. The ferritic or forged austeniticsteel will be modelled as an isotropic material.     

A new reagent for polypeptide synthesis: mu-oxo-bis-(tris-(dimethylamino)-phosphonium)-bis-tetrafluoroborate.

The products 1 and 2 (X = OTs) have been isolated from the reaction between hexamethylphosphortriamide and p-toluene sulfonic anhydride and the latter converted into μ-oxo-bis-[tris-(dimethylamino)-phosphonium]-bis-tetrafluoroborate 2 (X = BF₄). This is a practical reagent for the formation of the peptide link. Where racemisation is possible via oxazolone formation this can be decreased by the addition of 1-hydroxybenzotriazole or N-hydroxysuccinimide. These additives may also increase the efficiency of condensation at glycine and proline residues.     

Diphenylphosphinic mixed anhydrides in solid-phase peptide synthesis

Diphenylphosphinic mixed anhydrides have been evaluated for use in solid-phase peptide synthesis using a phenolic polystyrene support. These mixed anhydrides were successfully used for the preparation of an amino terminal fragment of “Bombesin like” peptide and rapid, efficient acylation was observed during the assembly of the peptide on the support. No evidence of disproportionation or wrong way opening were observed.