HRID1460820

反应详情

EQUATION

反应方程式

HRID 1460820 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

After adding 90.8 g of dicyclohexylcarbodiimide to a mixture of 150 g (0.400) of 4-chloromethyl-5-phenyl-2-(4-carboxy-2-nitrophenyl)-4-isoxazolin-3-one prepared in the above step and 600 ml of chloroform, the reaction was performed for 30 minutes at room temperature. Then, 97.4 g of 3-dodecyloxypropylamine was added dropwise to the reaction mixture and thereafter, the reaction was further performed for 5 hours. The reaction product was purified by a short column of silica gel and the product was recrystallized from acetonitrile to provide 78.0 g of the desired product with a yield of 33.4%. The melting point thereof was 110° C. to 111° C.

WORKUP

后处理

  1. waitthe reaction was further performed for 5 hours
  2. customThe reaction product was purified by a short column of silica gel
  3. customthe product was recrystallized from acetonitrile