反应详情

In an ice-bath, to a solution (4 mL) of the crude compound (0.84 mmol) obtained in Example 36b in tetrahydrofuran were added triethylamine (0.15 ml, 1.1 mmol) and ethyl chlorocarbonate (79 ml, 1.0 mmol), and the mixture was stirred at room temperature overnight. After confirmation of the termination of the reaction by TLC, the resulting salt was removed. The solvent was evaporated under reduced pressure. The resulting crude title compound was recrystallized (hexane-ethyl acetate) to give the title compound (180 mg, 54% in 2 steps) as colorless crystals.

1. customAfter confirmation of the termination of the reaction by TLC
2. customthe resulting salt was removed
3. customThe solvent was evaporated under reduced pressure
4. customThe resulting crude title compound was recrystallized (hexane-ethyl acetate)