HRID41589
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 stirred solution of (3-(pyrazin-2-yl)phenyl)methanol (200 mg, 1.08 mmol) in THF (5 mL), PBr3 (349 mg, 1.29 mmol) was added dropwise at 0° C. and stirred for 10 min. Then, the reaction mixture was refluxed for 3 h. The mixture was cooled to rt, poured into ice-cold saturated aqueous NaHCO3 solution (5 mL) and extracted with ethyl acetate (2×). The combined organic layers were washed with brine and dried over anhydrous Na2SO4, filtered and concentrated under reduced pressure to yield the title compound (200 mg, 75%). [TLC Rf=0.54 (ethyl acetate/hexane 50:50)].
WORKUP
后处理
- temperatureThen, the reaction mixture was refluxed for 3 h
- extractionextracted with ethyl acetate (2×)
- washThe combined organic layers were washed with brine
- dry with materialdried over anhydrous Na2SO4
- filtrationfiltered
- concentrationconcentrated under reduced pressure