HRID37223
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
A solution of the product of Step B (50 mg, 0.205 mmol) NBS (33 mg, 0.9 eq) and AIBN (5 mg, catalytic amount) in CCl4 (2 mL) was heated to reflux for 2 hours, and then concentrated in vacuo. The residue was chromatographed on a flash silica column (20×140 mm) eluted with 5% ethyl acetate/hexane to yield 32 mg (48%) of product (Rf =0.17, 5% ethyl acetate/hexane).
WORKUP
后处理
- temperatureto reflux for 2 hours
- concentrationconcentrated in vacuo
- customThe residue was chromatographed on a flash silica column (20×140 mm)
- washeluted with 5% ethyl acetate/hexane