反应详情

温度

160 °C

To a solution of 57 (135 mg, 0.5 mmol) in n-BuOH (3 mL) in a microwave vial was added 126 (184 mg, 0.75 mmol), then DIPEA (0.26 mL, 1.5 mmol) was added dropwise. The vial was sealed with a rubber septa and heated in the microwave for 90 min at 160° C. The solvent was evaporated under reduced pressure and the crude residue was taken up in DCM (5 mL) and MeOH (5 mL) and the solvent was again concentrated in vacuo. The residue was diluted in DMF (2 mL) and filtered to remove any undissolved solids. The filtrate was concentrated in vacuo. The residue was purified by reverse phase HPLC to afford 13 mg (6%) of I-46.

1. customThe vial was sealed with a rubber septa
2. customThe solvent was evaporated under reduced pressure
3. concentrationMeOH (5 mL) and the solvent was again concentrated in vacuo
4. additionThe residue was diluted in DMF (2 mL)
5. filtrationfiltered
6. customto remove any undissolved solids
7. concentrationThe filtrate was concentrated in vacuo
8. customThe residue was purified by reverse phase HPLC
9. customto afford 13 mg (6%) of I-46