反应详情

Lithium aluminium hydride (83.5 ml, 1M solution in THF) was added dropwise to a suspension of the subtitle product of step i) (7.1 g) in Et2O (180 ml) at a rate that maintained gentle reflux. Upon complete addition the reaction was stirred for 1.5 h. 15% sodium hydroxide solution was added dropwise until no effervescence was observed. The resulting white precipitate was filtered and the filtrate diluted with H2O (100 ml). The organics were removed in vacuo and the residue extracted with Et2O (100 ml). The organics were washed with 2M sodium hydroxide solution (150 ml), H2O (150 ml), brine (150 ml), dried (MgSO4) and concentrated in vacuo to afford the subtitle compound as a white crystalline solid. Yield: 5.5 g.

1. temperaturemaintained gentle reflux
2. additionUpon complete addition the reaction
3. filtrationThe resulting white precipitate was filtered
4. additionthe filtrate diluted with H2O (100 ml)
5. customThe organics were removed in vacuo
6. extractionthe residue extracted with Et2O (100 ml)
7. washThe organics were washed with 2M sodium hydroxide solution (150 ml), H2O (150 ml), brine (150 ml)
8. dry with materialdried (MgSO4)
9. concentrationconcentrated in vacuo