HRID132688
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- waitthe stirring was continued for 3 hr at RT
- washwashed with water
- dry with materialdried over Na2SO4
- concentrationconcentrated
- customPurification by flash chromatography (silica gel, 30% EtOAc in hexanes)