HRID46001

反应详情

EQUATION

反应方程式

HRID 46001 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

5

PROCEDURE

实验过程

To a degassed solution of 4-bromopyridine (1 equiv.), tert-butyl piperazine-1-carboxylate (16 mmol, 1.2 equiv.) and NaOtBu (3.4 equiv.) in toluene were added Pd(OAc)2 (2 mol %) and BINAP (1 mol %) and the resulting solution was refluxed for 3 h. The reaction mixture was cooled, diluted with ethyl acetate and given water and brine washes respectively. The organic layer was dried over sodium sulfate, the solvent removed in vacuo and the crude product purified by column chromatography (silica). Yield: 47%.

WORKUP

后处理

  1. temperaturethe resulting solution was refluxed for 3 h
  2. temperatureThe reaction mixture was cooled
  3. dry with materialThe organic layer was dried over sodium sulfate
  4. customthe solvent removed in vacuo
  5. customthe crude product purified by column chromatography (silica)