HRID1108548
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 0 °C
PROCEDURE
实验过程
A 100 mg portion of Boc-(D)-Arg(Cbz2)-Gly-Arg(Tos)-Thiazole, 1 mL of anisole and 4 drops of MeSEt were placed in HF-cleavage vessel and cooled under liquid N2. HF (10 mL) was then condensed into the reaction mixture and stirred at 0° C. for 1.25 h. HF was removed under vacuum to give a gum-like residue which was titrated with 20 mL of 50% Et2O-hexane and the organic wash removed by filtration. The gum residue was dissolved in 30 mL of 30% aq. HOAc and filtered through the above sintered funnel. The filtrate was lyophilized to give a powder which was purified by RP-HPLC to give 28 mg (60% yield) of (D)-Arg-Gly-Arg-thiazole. FAB-MS (M+H)+ =455.2
WORKUP
后处理
- customcondensed into the reaction mixture
- customHF was removed under vacuum
- customto give a gum-like residue which
- washthe organic wash
- customremoved by filtration
- dissolutionThe gum residue was dissolved in 30 mL of 30% aq. HOAc
- filtrationfiltered through the above sintered funnel
- customto give a powder which
- customwas purified by RP-HPLC