HRID13816
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 the product of Step C EXAMPLE 26 (300 mg) in THF (3.3 mL) was added isobutylamine (0.83 mL). The reaction stirred at room temperature overnight at which point LC/MS indicated incomplete reaction. The temperature was elevated to 50° C. for 6 hours at which point the reaction was diluted with EtOAc and washed with saturated aqueous NaHCO3 solution. The solution was concentrated and purified via flash chromatography on silica gel with a gradient elution of 0% to 15% EtOAc in hexane affording the title compound. HPLC/MS: 396.1 (M+1), 398.1 (M+3); Rt=4.77 min.
WORKUP
后处理
- customreaction
- waitThe temperature was elevated to 50° C. for 6 hours at which
- washwashed with saturated aqueous NaHCO3 solution
- concentrationThe solution was concentrated
- custompurified via flash chromatography on silica gel with a gradient elution of 0% to 15% EtOAc in hexane affording the title compound