反应详情

温度

20 °C

To a solution of 2,4-dimethoxy-benzylamine hydrochloride (1 eq.) and TEA (2 eq.) in DCM was added dropwise at 0° C. a solution of 3-chloro-propane-1-sulfonyl chloride (1 eq.) in DCM. The reaction was stirred at 20° C. for 20 h. The crude was diluted with DCM, washed twice with water, twice with aqueous HCl (0.1N) and twice with a saturated aqueous solution of NaHCO3. The organic layer was dried over MgSO4, filtered and concentrated under reduced pressure. The crude was purified by chromatography on silica gel (elution with heptane/EtOAc: 100/0 to 20/80) to afford 3-chloro-propane-1-sulfonic acid 2,4-dimethoxy-benzylamide.

1. washwashed twice with water, twice with aqueous HCl (0.1N) and twice with a saturated aqueous solution of NaHCO3
2. dry with materialThe organic layer was dried over MgSO4
3. filtrationfiltered
4. concentrationconcentrated under reduced pressure
5. customThe crude was purified by chromatography on silica gel (elution with heptane/EtOAc: 100/0 to 20/80)