反应详情

温度

120 °C

A solution of the above acetylpyrazolidine (50 mg, Step 1), water (0.25 mL), and TFA (0.15 mL) in acetonitrile (5 mL) was stirred at room temperature for 6 hours. The resultant mixture was concentrated under vacuum. Residual water and TFA was removed by co-evaporation with additional acetonitrile (3×5 mL). Without further purification, the residual oil was treated with 4-fluorobenzylamine (0.2 mL) in a mixture of methanol (1 mL) and toluene (8 mL) in a sealed tube was heated in an oil bath at 120° C. for 2 hours. The product mixture was concentrated under vacuum. The residue was dissolved in DMSO, and subjected to HPLC purification on C-18 stationary phase eluted with water/acetonitrile/TFA mobile phase. Collection and lyophilization of appropriate fractions provided the title compound.

1. concentrationThe resultant mixture was concentrated under vacuum
2. customResidual water and TFA was removed by co-evaporation with additional acetonitrile (3×5 mL)
3. customWithout further purification
4. additionthe residual oil was treated with 4-fluorobenzylamine (0.2 mL) in a mixture of methanol (1 mL) and toluene (8 mL) in a sealed tube
5. concentrationThe product mixture was concentrated under vacuum
6. dissolutionThe residue was dissolved in DMSO
7. customsubjected to HPLC purification on C-18 stationary phase
8. washeluted with water/acetonitrile/TFA mobile phase
9. customCollection and lyophilization of appropriate fractions