反应详情

A solution of 5.0 g of N2 -(6,7-dimethoxy-2-naphthalenesulfonyl)-L-arginyl-N-(2-ethylthioethyl)glycine tert-butyl ester in 10 ml of trifluoroacetic acid was stirred for 5 hours at room temperature. At the end of this period, the reaction mixture was evaporated to dryness. The residue was washed several times with dry diethyl ether and chromatographed on 80 ml of Daiaion® SK 102 ion exchange resin (200-300 mesh, H+ form, manufactured by Mitsubishi Chemical Industries Limited) packed in water, washed with water and eluted with ethanol-H2O-NH4OH (5:4:1). The main fraction eluted from the ethanol-H2O-NH4OH solution was evaporated to dryness to give a crystalline material. This was recrystallized from water to give 1.2 g of N2 -(6,7-dimethoxy-2-naphthalenesulfonyl)-L-arginyl-N-(2-ethylthioethyl) glycine, M.P. 171°-2° C.

1. customAt the end of this period, the reaction mixture was evaporated to dryness
2. washThe residue was washed several times with dry diethyl ether
3. customchromatographed on 80 ml of Daiaion® SK 102 ion exchange resin (200-300 mesh, H+ form, manufactured by Mitsubishi Chemical Industries Limited)
4. washwashed with water
5. washeluted with ethanol-H2O-NH4OH (5:4:1)
6. washThe main fraction eluted from the ethanol-H2O-NH4OH solution
7. customwas evaporated to dryness
8. customto give a crystalline material
9. customThis was recrystallized from water