反应详情

Triethylsilane (3 equivalents) was added to a solution of 85 in trifluoroacetic acid (2 mL per mmol). The mixture was stirred for 48 h at room temperature. The TFA was removed under vacuum and the crude product was taken up in AcOEt, washed with NaOH (2 M), brine, dried with Na2SO4, filtered and concentrated to give crude product. The residue was purified by HPLC. Yield: 46% for two steps. 1H-NMR (400 MHz, CDCl3): δ 1.35 (t, 3H), 2.26 (s, 3H), 2.69 (m, 2H), 2.78 (m, 2H), 4.31 (q, 2H), 6.55 (d, 1H), 7.08 (d, 2H), 7.22 (d, 2H), 8.86 (s broad, 1H) ppm.

1. customThe TFA was removed under vacuum
2. washwashed with NaOH (2 M), brine
3. dry with materialdried with Na2SO4
4. filtrationfiltered
5. concentrationconcentrated
6. customto give crude product
7. customThe residue was purified by HPLC