HRID1716279
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 a suspension of N-(2-bromo-pyridin-3-yl)-4-phenoxy-benzene-sulfonamide (0.38 g, 0.94 mmol) from step A and K2CO3 (0.39 g, 2.81 mmol) in dry DMF (10 mL) was added benzylbromide (0.13 mL, 1.13 mmol). The resulting mixture was heated at 80 C overnight. The cooled reaction was diluted with EtOAc and water. The aqueous layer was extracted with EtOAc (×3) and the combined organics were washed with water and brine, dried over anhydrous Na2SO4, and filtered through Celite. The filtrate was concentrated under the reduced pressure and purified by chromatography (silica gel, 25% EtOAc/hexanes). MS: 495, 497 (M+H)+.
WORKUP
后处理
- temperatureThe resulting mixture was heated at 80 C overnight
- customThe cooled reaction
- extractionThe aqueous layer was extracted with EtOAc (×3)
- washthe combined organics were washed with water and brine
- dry with materialdried over anhydrous Na2SO4
- filtrationfiltered through Celite
- concentrationThe filtrate was concentrated under the reduced pressure
- custompurified by chromatography (silica gel, 25% EtOAc/hexanes)