HRID1451513

反应详情

EQUATION

反应方程式

HRID 1451513 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

2-Bromobiphenyl (20.0 g, 86 mmol) in THF (85 ml) was dropwise added to a refluxing suspension of magnesium (2.1 g, 86 mmol) in THF (15 ml). The reaction mixture was refluxed for 18 h and an extra batch of 2-bromobiphenyl (2.0 g, 8.6 mmol) was added. The reaction mixture was refluxed for 2 h and cooled to 0° C. on an icebath. Ethyleneoxide (14.0 g, 0.32 mol) was was added. The reaction mixture was refluxed for 18 h, cooled to 0° C. and a saturated solution of ammonium chloride (100 ml) was dropwise added at this temperature. The reaction mixture was diluted with diethyl ether (100 ml) and concentrated hydrochloric acid was added until pH 2. The organic phase was separated, dried (MgSO4) and concentrated in vacuo. The residue was submitted to column chromatography on silica gel (800 ml) using heptane and ethyl acetate (7:3) as eluent to give 8.5 g of 2-(biphenyl-2-yl)ethanol as an oil.

WORKUP

后处理

  1. temperatureThe reaction mixture was refluxed for 18 h
  2. temperatureThe reaction mixture was refluxed for 2 h
  3. temperatureThe reaction mixture was refluxed for 18 h
  4. temperaturecooled to 0° C.
  5. additionwas added until pH 2
  6. customThe organic phase was separated
  7. dry with materialdried (MgSO4)
  8. concentrationconcentrated in vacuo