反应详情

To a solution of N-[7-(2-aminoethyl)-chroman-4-yl]-3-phenyl-3-(3-trifluoromethylbenzenesulfonylamino)-propionamide (Example 208, 50 mg, 0.09 mmol) in dry CH2Cl2 (8 mL) was added isobutyraldehyde (83 L, 0.9 mmol) and HOAc (1 drop). The resulting mixture was stirred at RT under N2 After 3 h, MS showed the formation of imine; NaBH4 (17 mg, 0.45 mmol) was then added. The resulting mixture was stirred for 18 h. Quenched with minimum amount of sat. NaHCO3. The organic layer was isolated, dried over MgSO4 and evaporated in vacuo. The crude product was purified by chromatography on silica gel. Elution with CH2Cl2:MeOH mixture (97:3) gave final compound. MS m/z: 660.31 (M+H). Calc'd. for Calc'd. for C35H44F3N3O4S-659.82.

1. stirringThe resulting mixture was stirred for 18 h
2. customQuenched with minimum amount of sat. NaHCO3
3. customThe organic layer was isolated
4. dry with materialdried over MgSO4
5. customevaporated in vacuo
6. customThe crude product was purified by chromatography on silica gel
7. washElution with CH2Cl2