反应详情

温度

90 °C

2-Hydroxy-4-[4-(3-hydroxy-prop-1-ynyl)-benzylamino]-benzoic acid methyl ester (22 mg; 0.07 mmol) was dissolved in THF/H2O (1 mL/0.25 mL) and LiOH was added (17 mg; 0.7 mmol). The reaction mixture was heated to 90° C. for 1 hour. THF was removed by evaporation and EtOAc (3 mL) and H2O (0.5 mL) was added. The organic phase was isolated, dried (Na2SO4), filtered, evaporated to dryness and purified by flash column chromatography (SiO2-PE80-100° C./EtOAc/CH3COOH=1:1:1%) to yield 3.6 mg (17%) of pure product.

1. customTHF was removed by evaporation and EtOAc (3 mL) and H2O (0.5 mL)
2. additionwas added
3. customThe organic phase was isolated
4. dry with materialdried (Na2SO4)
5. filtrationfiltered
6. customevaporated to dryness
7. custompurified by flash column chromatography (SiO2-PE80-100° C./EtOAc/CH3COOH=1:1:1%)