HRID475360

反应详情

EQUATION

反应方程式

HRID 475360 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
50 °C

PROCEDURE

实验过程

To a stirred solution of Example 32A (0.2 g, 0.49 mmol) in acetonitrile (4.0 mL) at room temperature was added iodotrimethysilane (0.11 mL, 0.75 mmol). The reaction mixture was stirred at 50° C. for 30 minutes and then concentrated under reduced pressure. The solid residue was washed with acetone and ether and filtered to provide titled compound. MS (CI) m/z 277 (M+1)+; 1H NMR (300 MHz, DMSO-d6) δ ppm 8.04 (d, 2H), 7.90 (bs, 2H NH2-DMSO solvent), 7.50 (d, 2H), 3.88 (s, 3H), 3.35-3.20 (m, 4H), 1.79-1.58 (m, 4H), 1.35 (s, 3H).

WORKUP

后处理

  1. concentrationconcentrated under reduced pressure
  2. washThe solid residue was washed with acetone and ether
  3. filtrationfiltered