Document Detail


In situ neutralization in Boc-chemistry solid phase peptide synthesis. Rapid, high yield assembly of difficult sequences.
MedLine Citation:
PMID:  1478777     Owner:  NLM     Status:  MEDLINE    
Abstract/OtherAbstract:
Simple, effective protocols have been developed for manual and machine-assisted Boc-chemistry solid phase peptide synthesis on polystyrene resins. These use in situ neutralization [i.e. neutralization simultaneous with coupling], high concentrations (> 0.2 M) of Boc-amino acid-OBt esters plus base for rapid coupling, 100% TFA for rapid Boc group removal, and a single short (30 s) DMF flow wash between deprotection/coupling and between coupling/deprotection. Single 10 min coupling times were used throughout. Overall cycle times were 15 min for manual and 19 min for machine-assisted synthesis (75 residues per day). No racemization was detected in the base-catalyzed coupling step. Several side reactions were studied, and eliminated. These included: pyrrolidonecarboxylic acid formation from Gln in hot TFA-DMF; chain-termination by reaction with excess HBTU; and, chain termination by acetylation (from HOAc in commercial Boc-amino acids). The in situ neutralization protocols gave a significant increase in the efficiency of chain assembly, especially for "difficult" sequences arising from sequence-dependent peptide chain aggregation in standard (neutralization prior to coupling) Boc-chemistry SPPS protocols or in Fmoc-chemistry SPPS. Reported syntheses include HIV-1 protease(1-50,Cys.amide), HIV-1 protease(53-99), and the full length HIV-1 protease(1-99).
Authors:
M Schnölzer; P Alewood; A Jones; D Alewood; S B Kent
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Publication Detail:
Type:  Journal Article; Research Support, Non-U.S. Gov't    
Journal Detail:
Title:  International journal of peptide and protein research     Volume:  40     ISSN:  0367-8377     ISO Abbreviation:  Int. J. Pept. Protein Res.     Publication Date:    1992 Sep-Oct
Date Detail:
Created Date:  1993-02-05     Completed Date:  1993-02-05     Revised Date:  2006-11-15    
Medline Journal Info:
Nlm Unique ID:  0330420     Medline TA:  Int J Pept Protein Res     Country:  DENMARK    
Other Details:
Languages:  eng     Pagination:  180-93     Citation Subset:  IM; X    
Affiliation:
Scripps Research Institute, La Jolla, CA.
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MeSH Terms
Descriptor/Qualifier:
Acetylation
Acyl Carrier Protein / chemical synthesis
Chromatography, High Pressure Liquid
Formic Acid Esters / chemistry*
Glutamine / chemistry
HIV Protease / chemical synthesis
Mass Spectrometry
Peptide Fragments / chemical synthesis
Peptides / chemical synthesis*
Polystyrenes*
Resins, Synthetic*
Stereoisomerism
Time Factors
Chemical
Reg. No./Substance:
0/Acyl Carrier Protein; 0/Formic Acid Esters; 0/HIV-1 protease (44-48); 0/HIV-1 protease (89-99); 0/Peptide Fragments; 0/Peptides; 0/Polystyrenes; 0/Resins, Synthetic; 0/t-butyloxycarbonyl group; 56-85-9/Glutamine; 66851-75-0/acyl carrier protein (65-74); EC 3.4.23.-/HIV Protease

From MEDLINE®/PubMed®, a database of the U.S. National Library of Medicine


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