反应详情

The product of Example XXXVI (14.0 g, 0.0436 m) was dissolved in EtOH (1.5 lit) and the pH was adjusted to 4 with methanolic HCl. A solution of NaBH3CN (18.0 g, 0.272 m) in MeOH (300 ml) was added. The pH was readjusted to 4 at 5 min intervals for 20 min. After this time, the pH remained at 4. The reaction mixture was stirred at ambient temperature for 2 hr. The solvent was removed and the residue slurried in H2O (250 ml) and treated with 1N NaOH until basic. The mixture was extracted with CH2Cl2 (2 × 200 ml). The organic extract was dried over Na2SO4, filtered, and the solvent removed to give a white solid; m.p. 102°-103° C.

1. waitintervals for 20 min
2. customThe solvent was removed
3. additionthe residue slurried in H2O (250 ml) and treated with 1N NaOH until basic
4. extractionThe mixture was extracted with CH2Cl2 (2 × 200 ml)
5. extractionThe organic extract
6. dry with materialwas dried over Na2SO4
7. filtrationfiltered
8. customthe solvent removed
9. customto give a white solid