HRID1734105

反应详情

EQUATION

反应方程式

HRID 1734105 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To 22.3 g of succinic acid, 24.0 g of 6-amidino-2-naphthyl 5-aminomethylfuran-2-carboxylate dihydrochloride and 790 mg of DMAP was added 240 ml of pyridine, and the mixture was stirred while cooling with ice. After 10 minutes, 25.9 g of DCC was added and the mixture was stirred for 3 hours while cooling with ice and then for 16 hours at room temperature. The precipitate was filtered off, and the filtrate was added in small portions into 2 l of ether and stirred at room temperature for 3 hours. After removing the supernatant by decantation, 1 l of acetone was added to the residue and stirred for 3 hours. The precipitate was collected by filtration to obtain 24.0 g of the intended product.

WORKUP

后处理

  1. temperaturewhile cooling with ice
  2. stirringthe mixture was stirred for 3 hours
  3. temperaturewhile cooling with ice
  4. waitfor 16 hours at room temperature
  5. filtrationThe precipitate was filtered off
  6. additionthe filtrate was added in small portions into 2 l of ether
  7. stirringstirred at room temperature for 3 hours
  8. customAfter removing the supernatant by decantation, 1 l of acetone
  9. additionwas added to the residue
  10. stirringstirred for 3 hours
  11. filtrationThe precipitate was collected by filtration