反应详情

The methyl 4-(((benzyloxycarbonyl)(methyl)amino)methyl)benzoate was dissolved in methanol, then LiOH (0.35 g, 14.7 mmol) was added. The resulting mixture was maintained at room temperature for 2 days. The mixture was adjusted to pH=1˜2 with 2N aqueous hydrochloric acid then extracted with ethyl acetate (50 mL×3). The combined organic layer was washed with brine, dried over anhydrous sodium sulfate and condensed under vacuum. The residue was purified by silica gel chromatography (petrol ether:ethyl acetate=10:1) to yield a white solid of 4-(((benzyloxycarbonyl)(methyl)amino)methyl)benzoic acid (1.25 g, 56.8%), LC-MS (ESI) m/z 300 [M+1]+.

1. extractionthen extracted with ethyl acetate (50 mL×3)
2. washThe combined organic layer was washed with brine
3. dry with materialdried over anhydrous sodium sulfate and condensed under vacuum
4. customThe residue was purified by silica gel chromatography (petrol ether:ethyl acetate=10:1)