HRID2175886

反应详情

EQUATION

反应方程式

HRID 2175886 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 4-cyclopropyl-5-vinyl-2-benzofuran-1(3H)-one (440 mg, 2.2 mmol) in 50 mL of DCM was slowly added mCPBA (1.14 g, 6.6 mmol) in 50 mL of DCM at 0° C. After warming to room temperature, the mixture was stirred for 12 hours. The mixture was washed with aqueous Na2SO3 until potassium iodide (KI) indicator paper did not change color. The organic layers were combined, washed with brine and then concentrated. The residue was purified via prep-TLC to give the title compound: 1H-NMR (400 MHz, CDCl3) δ ppm 7.77 (d, J=8.6 Hz, 1H), 7.39 (d, J=7.8 Hz, 1H), 5.39 (s, 2H), 4.43-4.45 (m, 1H), 3.26-3.28 (m, 1H), 2.68-2.70 (m, 1H), 1.94-2.01 (m, 1H), 1.08-1.12 (m, 2H), 0.65-0.75 (m, 2H).

WORKUP

后处理

  1. customat 0° C
  2. washThe mixture was washed with aqueous Na2SO3 until potassium iodide (KI) indicator paper
  3. washwashed with brine
  4. concentrationconcentrated
  5. customThe residue was purified via prep-TLC