反应详情

(4-Hydroxy-3,5-dimethoxy-phenyl)-acetic acid (9.5 g, 0.042 mmol) was added to methanol (260 mL) and sulfuric acid (8 mL). After completion of addition the reaction was heated at reflux overnight. The next day, the reaction mixture was cooled down and concentrated to yield a crude oil. The oil was re-dissolved in ethyl acetate, washed with water, brine, and dried over sodium sulfate, and filtered to be concentrated again. The crude material was purified using silica gel chromatography (50%:50% ethyl acetate:pentane) to yield the desired product (1.5 g, 75% yield based on recovered starting material).

1. additionAfter completion of addition the reaction
2. temperaturewas heated
3. temperatureat reflux overnight
4. temperatureThe next day, the reaction mixture was cooled down
5. concentrationconcentrated
6. customto yield a crude oil
7. washwashed with water, brine
8. dry with materialdried over sodium sulfate
9. filtrationfiltered
10. concentrationto be concentrated again
11. customThe crude material was purified