反应详情

温度

50 °C

2-methoxycarbonylmethyl-5-nitro-benzoic acid methyl ester (2.2 g, 8.8 mmol) was dissolved in MeOH (30 mL), then heated to 50° C. To the solution was added SnCl2 (5.89 g, 31 mmol) in batches. The reaction mixture was stirred at this temperture for 1 day. TLC monitored the reaction. After the reaction completed, the solvent was evaporated. To the residue was added ethyl acetate and base, adjusted pH to 8˜9, then filtered though celite and washed with ethyl acetate. The organic layer of the filtrate was collected and washed with water, dried over anhydrous Na2SO4 and concentrated to give 1.3 g of 5-amino-2-methoxycarbonylmethyl-benzoic acid methyl ester (18D).

1. customthe reaction
2. customthe solvent was evaporated
3. additionTo the residue was added ethyl acetate and base
4. filtrationfiltered though celite
5. washwashed with ethyl acetate
6. customThe organic layer of the filtrate was collected
7. washwashed with water
8. dry with materialdried over anhydrous Na2SO4
9. concentrationconcentrated