HRID1926591

反应详情

EQUATION

反应方程式

HRID 1926591 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
2.5 °C

PROCEDURE

实验过程

To a flask was added N-(5-nitro-2-methyl-pyrid-3-yl)-4-(pyrid-3-yl)-2-pyrimidinamine (18.0 g) and THF (200 mL) and the solution was cooled to 0-5° C. To the solution was added LiAlH4 (about 2.2 g in total) in several portions and the mixture was stirred for 2 hours at the same temperature. The reaction mixture was acidified to pH=5-6 using 1N HCl and then extracted with CH2Cl2 (2×100 mL ). The organic extracts were combined, dried, filtrated and concentrated to afford N-(5-amino-2-methylpyrid-3-yl)-4-(pyrid-3-yl)-2-pyrimidinamine (12 g).

WORKUP

后处理

  1. extractionextracted with CH2Cl2 (2×100 mL )
  2. customdried
  3. filtrationfiltrated
  4. concentrationconcentrated