HRID57666

反应详情

EQUATION

反应方程式

HRID 57666 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
120 °C

PROCEDURE

实验过程

3.25 g (16 mmol) of 4-amino-2-(methylsulfonyl)-1,3-thiazole-5-carbonitrile (Example 6A) were dissolved in 50 ml of DMSO, and 3.8 g (24 mmol) of N-Boc-ethylenediamine and 2.8 ml (16 mmol) of N,N-diisopropylethylamine were added. The mixture was stirred at 120° C. for 12 h. The reaction mixture was taken up in a mixture of ethyl acetate and water. The organic phase was washed with saturated aqueous sodium chloride solution, dried over magnesium sulfate and concentrated on a rotary evaporator. The crude product was triturated with acetonitrile and the precipitated crystals were filtered off with suction. This gave 2.5 g (55% of theory) of the product as a solid.

WORKUP

后处理

  1. washThe organic phase was washed with saturated aqueous sodium chloride solution
  2. dry with materialdried over magnesium sulfate
  3. concentrationconcentrated on a rotary evaporator
  4. customThe crude product was triturated with acetonitrile
  5. filtrationthe precipitated crystals were filtered off with suction