反应详情

To a solution of 1-(3-amino-propyloxy)-3,5-bis-(hydroxymethyl)-benzene (50 mg) in dimethylformamide (1 mL) was added 4-methyl-4-methyldisulfanyl-pentanoic acid (44 mg), N,N′-diisopropylcarbodiimide (35 mL) and 1-hydroxybenzotriazole hydrate (5.8 mg). After 15 h at room temperature, water was added to the reaction mixture and the aqueous solution was extracted twice with ethyl acetate. The combined organic solutions were washed with a saturated sodium chloride aqueous solution, dried over magnesium sulfate and concentrated in vacuo to a residue. The residue was purified by silica gel chromatography (Interchrom Puriflash 5 g column, SiOH 15-35 μm), eluted with methanol/dichloromethane, 5:95 to give 1-[3-(4-methyl-4-methyldisulfanyl-pentanoylamino)-propyloxy]-3,5-bis-(hydroxymethyl)-benzene (48 mg):

1. extractionthe aqueous solution was extracted twice with ethyl acetate
2. washThe combined organic solutions were washed with a saturated sodium chloride aqueous solution
3. dry with materialdried over magnesium sulfate
4. concentrationconcentrated in vacuo to a residue
5. customThe residue was purified by silica gel chromatography (Interchrom Puriflash 5 g column, SiOH 15-35 μm)
6. washeluted with methanol/dichloromethane, 5:95