反应详情

The solution of 11-3 (440 mg, 1.85 mmol), HATU (850 g, 2.23 mmol), HNMe2.HCl (150 g, 1.84 mmol) in THF (5 mL) was added DIPEA (600 mg, 4.63 mmol) dropwise at 0° C. The reaction temperature was allowed to raise room temperature and stirred overnight. The volatile was removed by evaporation. A white residue was obtained, which was quenched with 100 mL of water and extracted with DCM (50 mL×4). The combined organic layers were dried over anhydrous Na2SO4. After filtration and concentration, the residue was purified by silica gel chromatography (elution with petroleum:ethyl acetate: 1:1) to get 12-2 (324 mg, 53.5%) as a white solid. LCMS: calc 327.4 and found 328.1 [MH]+.

1. customThe volatile was removed by evaporation
2. customA white residue was obtained
3. customwhich was quenched with 100 mL of water
4. extractionextracted with DCM (50 mL×4)
5. dry with materialThe combined organic layers were dried over anhydrous Na2SO4
6. filtrationAfter filtration and concentration
7. customthe residue was purified by silica gel chromatography (elution with petroleum:ethyl acetate: 1:1)