HRID257819

反应详情

EQUATION

反应方程式

HRID 257819 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. temperatureto reflux for 2 hours
  2. concentrationconcentrated in vacuo
  3. customThe residue was chromatographed on a flash silica column (20×140 mm)
  4. washeluted with 5% ethyl acetate/hexane