反应详情

The above-obtained 2-(benzyloxymethyl)-3-bromo-4,6-bis(methoxymethoxy)benzoic acid (16 mg, 0.036 mmol) was dissolved in methanol (2 mL) and the obtained mixture was further added with 2.0 mol/L trimethylsilyldiazomethane-hexane solution (0.30 mL, 0.60 mmol) followed by stirring at a room temperature for 1 hour. After adding acetic acid (0.050 mL) to the reaction mixture, the solvent was evaporated under reduced pressure. The obtained residue was dissolved in ethanol (4 mL) and the obtained solution was added with concentrated hydrochloric acid (0.10 mL) followed by stirring at 60° C. for 1 hour. The reaction mixture was concentrated under reduced pressure and the obtained residue was purified by preparative thin-layer chromatography (chloroform/methanol=20/1) to obtain Compound 10 (11 mg, 82%).

1. customthe solvent was evaporated under reduced pressure
2. dissolutionThe obtained residue was dissolved in ethanol (4 mL)
3. additionthe obtained solution was added with concentrated hydrochloric acid (0.10 mL)
4. stirringby stirring at 60° C. for 1 hour
5. concentrationThe reaction mixture was concentrated under reduced pressure
6. customthe obtained residue was purified by preparative thin-layer chromatography (chloroform/methanol=20/1)