反应详情

To a 100 mL beaker equipped with a magnetic stir bar was charged methadone hydrochloride (3.0 g, 8.67 mmol) and water (30 g). Ammonium hydroxide (0.79 g, 22.6 mmol) was added to bring the pH to ˜9 (pH paper). The resulting solution was extracted with two 45 g portions of ethyl acetate and the combined organic layers were concentrated under reduced pressure at 40° C. The residue was dried under high vacuum to provide 2.2 g (82%) of a white solid which was analyzed by DSC (FIG. 1), FTIR (FIG. 2), PXRD (FIG. 3), and 1H-NMR (FIG. 4). The PXRD diffractogram was consisted with a crystalline product.

1. customTo a 100 mL beaker equipped with a magnetic stir bar
2. extractionThe resulting solution was extracted with two 45 g portions of ethyl acetate
3. concentrationthe combined organic layers were concentrated under reduced pressure at 40° C
4. customThe residue was dried under high vacuum