反应详情

A solution of 2,2-dimethylpropionic acid 2-{(S)-3-[2-((S)-2-aminopropionylamino)-5-fluorophenylamino]piperidin-1-yl}ethyl ester (200 mg, 0.49 mmol), in aqueous 6M HCl (8 mL) was refluxed for 30 min. After cooling to RT the volatiles were removed in vacuo and the resulting residue loaded in dioxane/water (1:1) onto an Isolute® SCX-2 cartridge. The cartridge was washed with dioxane/water (1:1), then dioxane and the product eluted with 10% 880 NH3 in dioxane. The fractions containing product were purified by column chromatography (Si—PCC, gradient 3-18% 2M NH3/MeOH in DCM) affording the title compound as a colourless gum (71.2 mg, 47%). LCMS (Method J): RT 0.39 min [M+H]+ 307.

1. customwere removed in vacuo
2. washThe cartridge was washed with dioxane/water (1:1)
3. washdioxane and the product eluted with 10% 880 NH3 in dioxane
4. additionThe fractions containing product
5. customwere purified by column chromatography (Si—PCC, gradient 3-18% 2M NH3/MeOH in DCM)