HRID2214980

反应详情

EQUATION

反应方程式

HRID 2214980 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2 g (6.13 mmol) of 2-amino-4-[4-(2-methoxyethoxy)phenyl]-6-sulphanylpyridine-3,5-dicarbonitrile and 2.68 g (12.26 mmol) of 4-(4-(chloromethyl)-1,3-thiazol-2-yl]morpholine are dissolved in dry DMF (50 ml), and 1.83 ml (12.26 mmol) of DBU are added. After 3 hours of stirring at RT, the solvent is removed using a rotary evaporator and the residue is purified by preparative HPLC (column: Kromasil 100 C18 250×20 mm, 10 μm; acetonitrile/water gradient: 3 minutes of 10% acetonitrile which is then, over a period of 30 minutes, increased to 80% acetonitrile; flow rate: 25 ml/min). This gives 1.70 g (55% of theory) of product.

WORKUP

后处理

  1. customthe solvent is removed
  2. customa rotary evaporator
  3. customthe residue is purified by preparative HPLC (column
  4. custom3 minutes of 10% acetonitrile which
  5. waitover a period of 30 minutes
  6. temperatureincreased to 80% acetonitrile