HRID57894

反应详情

EQUATION

反应方程式

HRID 57894 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
120 °C

PROCEDURE

实验过程

A mixture of 6-bromo-2-fluoro-3-methoxy-pyridine (2.030 mmol; 418.1 mg), tert-butyl N-[(3S)-3-piperidyl]carbamate (3.044 mmol; 609.7 mg), and N-Methylmorpholine (6.089 mmol; 622 mg; 0.676 mL) in 1-methyl-2-pyrrolidinone (5 mL) in a sealed pressure vial was heated at 120° C. overnight. The mixture was poured into water, and extracted with EtOAc. The organic layer was concentrated. The residue was purified on silica eluted with 0 to 40% EtOAc in Heptane to afford tert-butyl N-[(3S)-1-(6-bromo-3-methoxy-2-pyridyl)-3-piperidyl]carbamate (743.5 mg, 95%).

WORKUP

后处理

  1. extractionextracted with EtOAc
  2. concentrationThe organic layer was concentrated
  3. customThe residue was purified on silica
  4. washeluted with 0 to 40% EtOAc in Heptane