HRID1360690

反应详情

EQUATION

反应方程式

HRID 1360690 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
90 °C

PROCEDURE

实验过程

To a solution of 4-bromo-2,6-difluorobenzyl methanesulfonate (from Step A above) in DMF (400 mL) was added LiBr (28.8 g, 335 mmol) and heated to 90° C. for 45 minutes. The reaction was cooled to room temperature and diluted with EtOAc. The organic layer was washed with water (5×), brine (2×) dried over MgSO4, and concentrated in vacuo to yield a brown oil. The crude residue was purified via silica gel column chromatography (CH2Cl2/hexanes) to yield the title compound (24 g).

WORKUP

后处理

  1. temperatureThe reaction was cooled to room temperature
  2. washThe organic layer was washed with water (5×), brine (2×)
  3. dry with materialdried over MgSO4
  4. concentrationconcentrated in vacuo
  5. customto yield a brown oil
  6. customThe crude residue was purified via silica gel column chromatography (CH2Cl2/hexanes)