HRID908673

反应详情

EQUATION

反应方程式

HRID 908673 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
165 °C

PROCEDURE

实验过程

22 μl (128 μmol; 2 equivalents) of diisopropylethylamine, 21 mg (64 μmol; 1 equivalent) of 5-[(3-bromopropyl)amino]-2-methyl-1,3-benzothiazole-4,7-dione and a spatula tip's worth of sodium iodide are added to 23.6 mg (64 μmol) of 5-({3-[(4-methoxybenzyl)amino]propyl}amino)-2-methyl-1,3-benzothiazole-4,7-dione dissolved in 5 ml of acetonitrile. The reaction mixture is maintained under stirring under microwaves at 165° C. for 15 minutes, then the solvent is evaporated off under reduced pressure and the reaction residue is taken up in dichloromethane, followed by washing with 3 times 50 ml of water. The organic phases are combined, dried over magnesium sulphate and the solvent is evaporated off under reduced pressure. The expected product is purified by chromatography on a silica column (eluent: dichloromethane/methanol: 93/7) and obtained in the form of a red oil.

WORKUP

后处理

  1. temperatureThe reaction mixture is maintained
  2. customthe solvent is evaporated off under reduced pressure
  3. washby washing with 3 times 50 ml of water
  4. dry with materialdried over magnesium sulphate
  5. customthe solvent is evaporated off under reduced pressure
  6. customThe expected product is purified by chromatography on a silica column (eluent: dichloromethane/methanol: 93/7)
  7. customobtained in the form of a red oil