反应详情

A mixture of 5-cyano-6-(4-ethoxy-2-nitro-5-phenoxy-phenyl)-4-(tetrahydro-pyran-4-yl)-hex-5-enoic acid (160 mg, 0.33 mmol), 3,3-dimethylbutylamine (40 mg, 0.4 mmol), HBTU (155 mg, 0.4 mmol) and DIEA (150 μL) in DMF (10 mL) was stirred at room temperature overnight. Water was then added, and the resulting mixture was extracted with methylene chloride (3×). The organic layer was washed with brine, dried over Na2SO4, filtered and concentrated. The resulting crude mixture was purified by chromatography (silica gel, 20-50% ethyl acetate in heptane) to yield a yellow oil.

1. extractionthe resulting mixture was extracted with methylene chloride (3×)
2. washThe organic layer was washed with brine
3. dry with materialdried over Na2SO4
4. filtrationfiltered
5. concentrationconcentrated
6. customThe resulting crude mixture was purified by chromatography (silica gel, 20-50% ethyl acetate in heptane)
7. customto yield a yellow oil