反应详情

Lithium aluminium hydride (440 mg, 11.6 mmol) was suspended in abs. THF (50 mL) in argon, mixed in drops with a solution of the title compound of step 3 (1.54 g, 5.53 mmol) in abs. THF (20 mL) and boiled for 4 h with reflux. The batch was then hydrolysed with water (10 mL) at 10° C. and filtered off over diatomaceous earth. The THF was removed in a vacuum, the residue adjusted to pH 11 with 1N NaOH and extracted with ethyl acetate. The combined organic phases were dried over Na2SO4, concentrated to low volume in a vacuum and the remaining residue was purified by flash chromatography with MeOH+2% NH3.

1. temperaturewith reflux
2. filtrationhydrolysed with water (10 mL) at 10° C. and filtered off over diatomaceous earth
3. customThe THF was removed in a vacuum
4. extractionextracted with ethyl acetate
5. dry with materialThe combined organic phases were dried over Na2SO4
6. concentrationconcentrated to low volume in a vacuum
7. customthe remaining residue was purified by flash chromatography with MeOH+2% NH3