反应详情

A mixture of 38 (0.08 g, 0.19 mmol), Zn dust (0.16 g, 2.45 mmol) and NH4Cl (g, mmol) in a mixture of CH2Cl2/MeOH (1:4, 20 mL) was stirred at room temperature for 3 h. The mixture was filtered and the filtrate was concentrated to dryness under reduced pressure. 2N NaOH (30 mL) was added to the residue and the mixture was extracted with CH2Cl2 (2×20 mL). The combined CH2Cl2 portion was washed with H2O (30 mL) and dried (Na2SO4). Removal of the solvent under reduced pressure afforded 0.06 g (84%) of 39 as a white solid, mp 237-240° C. (EtOAc/n-hexanes.

1. filtrationThe mixture was filtered
2. concentrationthe filtrate was concentrated to dryness under reduced pressure
3. addition2N NaOH (30 mL) was added to the residue
4. extractionthe mixture was extracted with CH2Cl2 (2×20 mL)
5. washThe combined CH2Cl2 portion was washed with H2O (30 mL)
6. dry with materialdried (Na2SO4)
7. customRemoval of the solvent under reduced pressure