反应详情

H2SO4 (25 mL, 296 mmol) was cooled to 0° C. and treated with P2O5 (10 g, 70 mmol). The mixture was brought to room temperature and added to diethyl 2-(4-(3-(trifluoromethyl)phenyl)-tetrahydro-2H-pyran-4-carbonyl)malonate (4.27 g, 10 mmol). The reaction mixture was then stirred for 1.5 hours. Ice (H2O) was added, and the aqueous mixture was extracted with EtOAc (2×). The combined organic layers were washed with water (2×) and brine, dried (MgSO4), and concentrated in vacuo to give the crude compound as a brown oil. The crude oil was purified by silica flash chromatography (0-100% DCM/hexane) to give the desired compound as a white solid (1.32 g). MS (m/e)=371.2 (M+H)+.

1. customwas brought to room temperature
2. additionIce (H2O) was added
3. extractionthe aqueous mixture was extracted with EtOAc (2×)
4. washThe combined organic layers were washed with water (2×) and brine
5. dry with materialdried (MgSO4)
6. concentrationconcentrated in vacuo
7. customto give the crude compound as a brown oil
8. customThe crude oil was purified by silica flash chromatography (0-100% DCM/hexane)