反应详情

温度

12.5 °C

A suspension of 5-[4-[(carbomethoxy)methoxy]benzyl]thiazolidine-2,4-dione obtained by following a procedure described in any of Examples 23-24 (135 g, 0.46 M) and water (540 ml, 4 times w/v) was taken in a round bottom flask fitted with a mechanical stirrer. Aq. sodium hydroxide solution (37 g of NaOH in 135 ml of water) was added slowly over a period of 5-10 minutes at 20-25° C. Stirring was continued at ambient temperature for a period of 2-3 h, while monitoring the reaction by TLC. After the completion of the reaction, the pH of the reaction mixture was adjusted to 2 using conc. HCl (temp. raises to 40-45° C.) and allowed to attain room temperature. The mass was cooled to 10-15° C. and the solid thus obtained was filtered and dried at 60-70° C. under 1-2 mm Hg of vacuum to afford 5-[4-[(carboxy)methoxy]benzyl]thiazolidine-2,4-dione (121 g, Y=99%, P=99.2%).

1. customobtained
2. customwas taken in a round bottom flask
3. customfitted with a mechanical stirrer
4. customthe reaction by TLC
5. customAfter the completion of the reaction
6. customto attain room temperature
7. customthe solid thus obtained
8. filtrationwas filtered
9. customdried at 60-70° C. under 1-2 mm Hg of vacuum