HRID132688

反应详情

EQUATION

反应方程式

HRID 132688 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

4

PROCEDURE

实验过程

To compound 1L (480 mg, 1.4 mmol) was added 7 mL of 10% TFA/CH2Cl2 solution at RT, and stirred at 4 hr. A 7 mL toluene was added to the reaction mixture, and concentracted. It was dissolved in 5 mL of CH2Cl2, a solution of PyBrop (1.2 g, 2.5 mmol) and compound 1G (210 mg, 1 mmol) in 3 mL of THF were added followed by iPr2NET (520 μL, 3 mmol), and the stirring was continued for 3 hr at RT. It was concentracted, dissolved in EtOAc, washed with water, dried over Na2SO4, and concentrated. Purification by flash chromatography (silica gel, 30% EtOAc in hexanes) provided the title compound (220 mg). MS (ES) m/z 435 [M+H]+.

WORKUP

后处理

  1. waitthe stirring was continued for 3 hr at RT
  2. washwashed with water
  3. dry with materialdried over Na2SO4
  4. concentrationconcentrated
  5. customPurification by flash chromatography (silica gel, 30% EtOAc in hexanes)