反应详情

温度

0 °C

117.4 mg of N-hydroxysuccinimidyl iodoacetate in solution in 3 ml of DCM are added to 100 mg of 3-(2-{2-[2-(2-aminoethoxy)ethoxy]ethoxy}ethoxy)propanoic acid. After 2 h at AT, 330 μl of MeOH are added and the mixture is cooled to 0° C. 360 μl of a 2M solution of trimethylsilyldiazomethane in hexane are added. After 1 h, the mixture is neutralized by addition of 50 μl of acetic acid and then a saturated aqueous NaHCO3 solution is added until pH=8 is obtained. The organic phase is dried over MgSO4 and concentrated under RP, and the residue is purified by flash chromatography on silica (Interchrom Puriflash Silica 15/35U 10G) using a gradient from 0 to 10% of methanol in DCM. 132 mg of methyl 3-[2-(2-{2-[2-(2-iodoacetylamino)ethoxy]ethoxy}ethoxy)ethoxy]propanoate are thus obtained.

1. customis obtained
2. dry with materialThe organic phase is dried over MgSO4
3. concentrationconcentrated under RP
4. customthe residue is purified by flash chromatography on silica (Interchrom Puriflash Silica 15/35U 10G)