反应详情

Acid Intermediate 1I (0.62 g, 1.79 mmol) was dissolved in DMF and L-tert-Leucine methylamide (0.31 g, 2.14 mmol) was added followed by DIEA (0.94 mL, 5.37 mmol). The resulting mixture was stirred for 20 minutes, HBTU (0.75 g, 1.97 mmol) was added in one portion and the mixture was stirred overnight. The mixture was diluted with water and extracted with ethyl acetate. The organic layer was washed successively with water, then brine, and dried over anhydrous Na2SO4, filtered and concentrated. The residue was purified by normal phase chromatography, eluting with a 0-10% methanol/DCM gradient to provide product Intermediate 1J as an off-white solid (0.68 g, 80%).

1. stirringthe mixture was stirred overnight
2. extractionextracted with ethyl acetate
3. washThe organic layer was washed successively with water
4. dry with materialbrine, and dried over anhydrous Na2SO4
5. filtrationfiltered
6. concentrationconcentrated
7. customThe residue was purified by normal phase chromatography
8. washeluting with a 0-10% methanol/DCM gradient