反应详情

In a 500 mL round bottom flask equipped with a reflux condenser 11.3 g (0.0357 mol) diethyl 2,3-dihydro-2-(hydroxymethyl)thieno[3,4-b][1,4]dioxine-5,7-dicarboxylate was combined with 12.0 g (0.214 mol) potassium hydroxide in 250 mL water. The reactin mixture was refluxed and the progress of the reaction tracked by TLC. Upon completion of the hydrolysis the reaction was concentrated to ˜100 mL. The mixture was cooled to 0 C then acidified with concentrated HCl. After allowing to warm to room temperature overnight the white solid was filtered and washed with a small amount of water. Drying under high vacuum gave 8.5 g (90%) of product as a white solid. Structure and purity were confirmed by 1H/13C NMR and LC-MS.

1. customUpon completion of the hydrolysis the reaction
2. concentrationwas concentrated to ˜100 mL
3. temperatureThe mixture was cooled to 0 C
4. filtrationwas filtered
5. washwashed with a small amount of water
6. customDrying under high vacuum