HRID63592

反应详情

EQUATION

反应方程式

HRID 63592 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

To a solution of 4-(4-((1,2,4-oxadiazol-3-yl)methyl)piperazin-1-yl)-5-chloro-3-nitropyridin-2-amine (50.0 mg, 0.147 mmol) and 1,3-dimethyl-1H-pyrazole-4-carbaldehyde (19.2 mg, 0.155 mmol) in EtOH (3.4 mL) was added 1M Na2S2O4 (0.588 mL, 0.588 mmol, freshly prepared) and the solution was heated to 80° C. and stirred for 15 h whilst being open to air. Once cooled, the reaction was evaporated in vacuo and the residue dry loaded onto silica. Purification was accomplished by flash chromatography on silica gel (2×14) eluting with MeOH/CH2Cl2 (5-7.5%) to yield the title compound (26 mg, 43%) as a pale yellow solid.

WORKUP

后处理

  1. customfreshly prepared) and the solution
  2. temperatureOnce cooled
  3. customthe reaction was evaporated in vacuo
  4. customthe residue dry
  5. customPurification
  6. washeluting with MeOH/CH2Cl2 (5-7.5%)