HRID1518524

反应详情

EQUATION

反应方程式

HRID 1518524 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of N-(2,3-difluorophenyl)-3-nitropyridin-4-amine in 200 mL of methanol under an atmosphere of nitrogen was added 10% Pd/C (0.75 g). The atmosphere was replaced with hydrogen gas and the reaction mixture stirred under balloon pressure for 14 hours at RT. The reaction mixture was filtered over Celite which was washed with methanol (3×30 mL). The filtrate was concentrated in vacuo to give a brown solid. The crude product was triturated with petroleum ether (3×50 mL) to afford N4-(2,3-difluorophenyl)pyridine-3,4-diamine (4.0 g, 90% yield) as light brown solid; LC-MS: 222.2 (M+H).

WORKUP

后处理

  1. filtrationThe reaction mixture was filtered over Celite which
  2. washwas washed with methanol (3×30 mL)
  3. concentrationThe filtrate was concentrated in vacuo
  4. customto give a brown solid
  5. customThe crude product was triturated with petroleum ether (3×50 mL)