反应详情

To a solution of 4-[2-(2,6-diethylphenyl)-4-methoxy-6-methylpyrimidin-5-yl]heptan-4-ol (0.6 g, 1.7 mmol) in anhydrous pyridine (10 mL) is added 1.5 mL of SOCl2 dropwise under nitrogen. The reaction mixture is stirred at room temperature for 3 h, quenched with a saturated aqueous NaHCO3 solution and extracted with DCM. The organic layer is washed with water, brine, dried over Na2SO4, and concentrated. The residue is purified by flash chromatography eluting with 10% EtOAc-hexanes to afford the title compound. 1H NMR (300 MHz, CDCl3): δ 7.24-7.29 (m, 1H), 7.13 (d, J=9 Hz, 2H), 5.39 (t, J=7.5. Hz, 1H), 3.91 (s,3H), 2.46 (s,3H),2.24-2.43 (m, 6H), 1.28-1.33 (m,4H), 1.10 (q, J=7.8, 4.8 Hz, 6H), 0.91 (t, j=7.2 Hz, 6H); LC-MS found 352 (MH+).

1. customquenched with a saturated aqueous NaHCO3 solution
2. extractionextracted with DCM
3. washThe organic layer is washed with water, brine
4. dry with materialdried over Na2SO4
5. concentrationconcentrated
6. customThe residue is purified by flash chromatography
7. washeluting with 10% EtOAc-hexanes