反应详情

A mixture of 2,6-dimethoxybenzoic acid (102 mg, 0.56 mmol), dimethylamine hydrochloride (91 mg, 1.12 mmol), 2-(1H-benzotriazole-1-yl)-1,1,3,3-tetramethyluronium tetrafluoroborate (234 mg, 0.73 mmol) and diisopropylethylamine (390 μL, 2.24 mmol) in DMF (1 mL) was stirred at ambient temperature overnight. The reaction mixture was taken up in ethyl acetate (50 mL) and aqueous. NaHCO3(50 mL). The organic phase was washed with brine (2×50 mL), dried (MgSO4), filtered and concentrated under reduced pressure. The residue was purified on silica gel eluting with ethyl acetate to provide titled compound (66 mg). MS (APCI(+)) m/e 210 (M+H)+.

1. washThe organic phase was washed with brine (2×50 mL)
2. dry with materialdried (MgSO4)
3. filtrationfiltered
4. concentrationconcentrated under reduced pressure
5. customThe residue was purified on silica gel eluting with ethyl acetate