N6-[叔丁氧羰基]-N2-[苄氧羰基]-D-赖氨酸琥珀酰亚胺基酯

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 8.8 Grams (20 mM) of H-Gly-Arg-CHA.2HCl was dissolved in 21.5 ml of DMF, to this solution was added 5.1 ml (40 mM) of NEM. To the mixture was further added with 9.6 g (20 mM) of Z-D-Lys(BOC)-OSu and reacted at room temperature for 18 hours. After the reaction was completed, the DMF was removed by evaporation under a reduced pressure and the residue obtained was dissolved in MeOH and reprecipitated in 1 liter of AcOEt. The crystals precipitated were collected by filtration and dried to obtain 14.9 g (97.4%) of Z-D-Lys(BOC)-Gly-Arg-CHA.HCl. Rf1 =0.50. Melting point: 207.5° C. (decomposed). [α]D20 -8.0 (C=0.5, MeOH) was added 5.1 ml (40 mM) of NEM reacted at room temperature for 18 hours the DMF was removed by evaporation under a reduced pressure the residue obtained reprecipitated in 1 liter of AcOEt The crystals precipitated were collected by filtration dried