1,2-Dichloroethane → HCID 131736683, compound

Participants

Reaction Conditions

Reaction Steps

1.05 equivalents of Boc-Ile-Leu-OH (Mw=344.4) and 1.10 equivalents of HOOBt (Mw=163.13) are added to a cold (0±5° C.) solution of 1.00 equivalent of 3HCl.H-Arg-Trp-Pro-Trp-Trp-Pro-Trp-Arg-Arg-Lys(Boc)-NH2 (Mw=1652.9; purity=89.0%) in DMA and CH2Cl2. 1.20 equivalents of EDC(N-(3-dimethylaminopropyl)-N-ethylcarbodiimide; Mw=191.7; purity=100.0%) was then added to the reaction mixture which was further stirred at 0±5° C. for about 4 hours, then at least 8 hours at room temperature. After the completion of the reaction had been checked by HPLC, the reaction mixture was diluted with a CH2Cl2/iso-butanol mixture (8/2), and washed with a 5% (weight) aqueous NaCl solution+HCl (0.3 eq.). After concentration of the organic layer, the residual oil was precipitated by slowly pouring into cold (0±5° C.) acetonitrile. After stirring at least for 30 min at 0±5° C., the suspension was filtered and washed twice with cold MTBE. The precipitate was dried at 40±5° C. An off white solid was finally obtained.

Provenance & Evidence