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温度

0 °C

5 g (15.8 mmol) of 3-[2-(4-chlorophenoxy)phenyl]-1-methylpyrrolidine-2,4-dione (compound IVb) was dissolved in a mixture of 150 mL of tetrahydrofuran and 15 mL of water. The solution was cooled to 0° C., and 4.3 g of potassium borohydride were added slowly, keeping the temperature below 10° C. The resulting solution was stirred at 0° C. for 6 hours. Then, a saturated solution of ammonium chloride was added, and the pH was adjusted to 3 with HCl 2 M. 100 mL of ethyl acetate were added. The organic phase was extracted, washed with saturated sodium bicarbonate and with water, dried and concentrated under vacuum, to obtain 4.5 g of 3-[2-(4-chlorophenoxy)phenyl]-4-hydroxy-1-methylpyrrolidine-2-one (compound XIIIb) as a sticky solid. Yield: 89.6%.

1. customthe temperature below 10° C
2. extractionThe organic phase was extracted
3. washwashed with saturated sodium bicarbonate and with water
4. customdried
5. concentrationconcentrated under vacuum