反应详情

温度

70 °C

To the title compound of step 2 (29.00 g, 136.79 mmol) and N(CH3)4Cl (22.47 g, 205.19 mmol) in anhydrous MeCN (300 mL), was added POCl3 (123.93 g, 820.74 mmol). The mixture was stirred at r.t. for 30 min and at 70° C. for 1 h. After concentration under vacuum, EA extractive work up and silica gel chromatography (PE: EA=50:1-5:1) gave the title compound (20 g, 63.6% yield) as a white solid. 1H NMR (CDCl3, 400 MHz) δ 8.16 (s, 1H), 3.95 (d, J=6.8 Hz, 2H), 2.56 (s, 3H), 1.33-1.28 (m, 1H), 0.72-0.70 (m, 2H), 0.41-0.37 (m, 2H). LCMS: 230.9 (M+1)+

1. concentrationAfter concentration under vacuum, EA extractive work up