HRID335862
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 solution of 8-bromo-2-chloro-4-nitro-10H-chromeno[3,2-b]pyridin-10-one (80 mg, 0.225 mmol) in 0.8 mL of DMF at 0° C. was added tetrabutylammonium fluoride (1M in THF, 0.45 mL, 0.450 mmol) dropwise. After 15 minutes, the reaction was quenched with saturated NH4Cl (20 mL) and extracted with ethyl acetate (2×10 mL). The combined organics were dried over sodium sulfate, filtered and evaporated to dryness. Purification of the crude residue by column chromatography (SiO2, CH2Cl2 to CH2Cl2/EA=100:3) gave 8-bromo-2-chloro-4-fluoro-10H-chromeno[3,2-b]pyridin-10-one as an off white solid.
WORKUP
后处理
- customthe reaction was quenched with saturated NH4Cl (20 mL)
- extractionextracted with ethyl acetate (2×10 mL)
- dry with materialThe combined organics were dried over sodium sulfate
- filtrationfiltered
- customevaporated to dryness
- customPurification of the crude residue by column chromatography (SiO2, CH2Cl2 to CH2Cl2/EA=100:3)