反应详情

The product of Example 48 (200 mg, 0.45 mmol) was combined and stirred with 5 mL of a 2M solution of ethylamine in THF. After 5 min the solvents were removed in vacuo, and the residue was partitioned between EtOAc and H2O. The organic phase was washed with H2O, satd aq NaCl, dried over anhyd Na2SO4, filtered and evaporated to give the crude product. Flash chromatography with 0-2% EtOAc/CH2Cl2 followed by recrystallization from CH2Cl2/hexane gave the product as a white-crystalline solid. mp 195-196°, LC MS m/z=411 (MH+) Retention time=2.4 min.

1. customAfter 5 min the solvents were removed in vacuo
2. customthe residue was partitioned between EtOAc and H2O
3. washThe organic phase was washed with H2O
4. dry with materialdried over anhyd Na2SO4
5. filtrationfiltered
6. customevaporated
7. customto give the crude product
8. customFlash chromatography with 0-2% EtOAc/CH2Cl2 followed by recrystallization from CH2Cl2/hexane