HRID1527125

反应详情

EQUATION

反应方程式

HRID 1527125 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To the solution of tert-butyl 4-(1-aminoethyl)piperidine-1-carboxylate (5 g, 21.9 mmol) in ethanol (50 ml) were added 5-bromo-2,4-dichloropyrimidine (5.97 g, 26.3 mmol), and N-ethyl-N-isopropylpropan-2-amine (8.48 g, 65.7 mmol). The resulting mixture was stirred at room temperature overnight. The reaction mixture was concentrated in vacuum, and the crude product was added to water (100 ml). The aqueous layer was extracted with ethyl acetate (50 mL×4) and organic layer was dried over sodium sulfate and concentrated to give crude product tert-butyl 4-(1-((5-bromo-2-chloropyrimidin-4-yl)amino)ethyl)piperidine-1-carboxylate (7 g, yield: 97.2%) as a yellow oil. LRMS (M+H+) m/z: calcd 418. found 419.

WORKUP

后处理

  1. concentrationThe reaction mixture was concentrated in vacuum
  2. additionthe crude product was added to water (100 ml)
  3. extractionThe aqueous layer was extracted with ethyl acetate (50 mL×4) and organic layer
  4. dry with materialwas dried over sodium sulfate
  5. concentrationconcentrated