反应详情

To the compound prepared in Example 1 (0.100 g) in 5 mL of DCM, 1.0 mL of DMF and N,N-diisopropylethylamine (DIEA) (0.072 g) was added the HATU (0.164 g) and stirred for 30 minutes. To the activated ester was added the compound prepared in Example 13 (0.15 g) and stirred for 1 hour. The reaction mixture was diluted with water, extracted with additional DCM, and the organic layer was washed with water, brine and dried over anhydrous Na2SO4. The DCM layer was filtered and concentrated, and the crude was chromatographed on silica gel using 10:1 DCM:MeOH to give the title compound (0.2 g) having the following physical data.

1. stirringstirred for 1 hour
2. extractionextracted with additional DCM
3. washthe organic layer was washed with water, brine
4. dry with materialdried over anhydrous Na2SO4
5. filtrationThe DCM layer was filtered
6. concentrationconcentrated
7. customthe crude was chromatographed on silica gel using 10:1 DCM