HRID1431380

反应详情

EQUATION

反应方程式

HRID 1431380 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a stirring solution of 4-(5-morpholino-3-nitropyridin-2-yl)morpholine (1.22 g, 4.15 mmol; described herein) and EtOAc (50 mL) was added tin(II) chloride dihydrate (4.52 g, 20.7 mmol). The mixture was stirred at rt for ten min, refluxed for 2 h, and then cooled to rt. A solid was removed by filtration and both this and the EtOAc solution were washed with water and brine. The combined aq. portions were basified with 1M NaOH and the product extracted with EtOAc, dried (magnesium sulfate), and concentrated, affording 2,5-dimorpholinopyridin-3-amine as a beige solid. Mass Spectrum (ESI) m/e=265.2 (M+1).

WORKUP

后处理

  1. temperaturerefluxed for 2 h
  2. temperaturecooled to rt
  3. customA solid was removed by filtration
  4. washboth this and the EtOAc solution were washed with water and brine
  5. extractionthe product extracted with EtOAc
  6. dry with materialdried (magnesium sulfate)
  7. concentrationconcentrated