HRID429382

反应详情

EQUATION

反应方程式

HRID 429382 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Into a solution of n-butyl lithium (165 ml, 264 mmol) in butyl ether (250 ml) at −78 degrees under nitrogen was added 3-bromopyridine (25.4 ml, 264 mmol). After 1 h, added diethylmethoxyborane (52 ml, 396 mmol). The mixture was allowed to warm to room temperature. After 16 h, added water and brine, separated organic layer, dried over sodium sulfate, then concentrated. The resulting slurry was dissolved in isopropanol (500 ml), cooled and the product isolated by filtration give diethyl(3-pyridyl)borane (29.8 g).

WORKUP

后处理

  1. waitAfter 16 h
  2. customseparated organic layer
  3. dry with materialdried over sodium sulfate
  4. concentrationconcentrated
  5. dissolutionThe resulting slurry was dissolved in isopropanol (500 ml)
  6. temperaturecooled
  7. customthe product isolated by filtration