HRID892199
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 [2-(3-hydroxymethyl-phenoxymethyl)-6-methyl-phenoxy]-acetonitrile (230 mg, 0.81 mmol, example 75) in THF (3 mL) is added Ph3P (233 mg, 0.89 mmol) and stirred until homogeneous. Cooled solution to 0° C. then added portionwise NBS (151 mg, 0.85 mmol) and let stir 45 min. Concentrated reaction mixture under reduced pressure. The residue is purified by flash chromatography (silica, 40% CH2Cl2 in hexanes) to give the title compound as a white crystalline solid. MS (EI) 345, 347 (M)+, Br pattern.
WORKUP
后处理
- stirringlet stir 45 min
- concentrationConcentrated
- customreaction mixture under reduced pressure
- customThe residue is purified by flash chromatography (silica, 40% CH2Cl2 in hexanes)