HRID1504762

反应详情

EQUATION

反应方程式

HRID 1504762 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
200 °C

PROCEDURE

实验过程

6-Chloropyridin-2-amine (244 mg, 1.90 mmol) and morpholine (0.827 mL, 9.49 mmol) were combined and heated for 2 hr at 200° C. via microwave irradiation. The reaction mixture was diluted with saturated aqueous ammonium chloride and DCM. The organics were separated, dried over sodium sulfate, and concentrated under reduced pressure. The residue was purified by silica gel chromatography (10-80% acetone/hexanes, linear gradient) to afford 6-(morpholin-4-yl)pyridin-2-amine. MS ESI calc'd. for C9H14N3O [M+H]+ 180. found 180. 1H NMR (500 MHz, CDCl3) δ 7.29 (t, J=7.9 Hz, 1H), 5.99 (d, J=8.1 Hz, 1H), 5.91 (d, J=7.8 Hz, 1H), 3.82-3.75 (m, 4H), 3.46-3.38 (m, 4H).

WORKUP

后处理

  1. customThe organics were separated
  2. dry with materialdried over sodium sulfate
  3. concentrationconcentrated under reduced pressure
  4. customThe residue was purified by silica gel chromatography (10-80% acetone/hexanes, linear gradient)