HRID1396874

反应详情

EQUATION

反应方程式

HRID 1396874 的结构方程式

CONDITIONS

反应条件

温度
225 °C

PROCEDURE

实验过程

6-Chloro-2-pyridinamine (1 g, 7.78 mmol) was dissolved in morpholine (6.80 ml, 78 mmol) and heated to 225° C. in a microwave reactor for 60 minutes (˜400 W; 5 mbar). The reaction was cooled to rt and concentrated. The crude product was taken up in DCM (50 mL). After filtration of white solids the crude product was concentrated and purified by silica gel column chromatography eluting with 20-50% EtOAc/hexanes to afford 1 g (5.58 mmol, 72%) of the title compound as a pale yellow solid. LC/MS: (M+H)+: 179.9.

WORKUP

后处理

  1. temperatureThe reaction was cooled to rt
  2. concentrationconcentrated
  3. filtrationAfter filtration of white solids the crude product
  4. concentrationwas concentrated
  5. custompurified by silica gel column chromatography
  6. washeluting with 20-50% EtOAc/hexanes