HRID1177509

反应详情

EQUATION

反应方程式

HRID 1177509 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
115 °C

PROCEDURE

实验过程

A slurry of N-(3,6-dichloropyridin-2-yl)pivalamide (1.83 g, 7.41 mmol) in 75 mL 5N aq HCl with water cooled reflux pyridine was heated in a 115° C. bath overnight, to give a clear yellow solution. The reaction mixture was cooled and poured onto ice, and was basified with 10 N NaOH. The resulting white precipitate was extracted with DCM, and the combined organics were dried over anhydrous sodium sulfate, filtered, and concentrated in vauco to give 3,6-dichloropyridin-2-amine as an off-white solid. MS (ESI) m/z: calculated: 162.0; Observed: 163.0 (M++1).

WORKUP

后处理

  1. customto give a clear yellow solution
  2. temperatureThe reaction mixture was cooled
  3. additionpoured onto ice
  4. extractionThe resulting white precipitate was extracted with DCM
  5. dry with materialthe combined organics were dried over anhydrous sodium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated in vauco