HRID1263002

反应详情

EQUATION

反应方程式

HRID 1263002 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 2.4 g of phenylacetic acid in 50 ml of anhydrous pyridine, while being cooled and stirred, was added 4.4 g of DCC. After 30 minutes, to the mixture was added 5.0 g of 6-amidino-2-naphthol methanesulfonate. The mixture was stirred at room temperature for 24 hours, mixed with ethyl ether, and the precipitate was collected by filtration. The precipitate was dissolved in DMF and the insolubles were filtered off. The filtrate containing the DMF-soluble substances was mixed with ethyl ether, the resulting precipitate was collected by filtration and recrystallized from a mixture of DMF and ethyl ether to obtain 3.0 g of a white powder of 6-amidino-2-naphthyl phenylacetate methanesulfonate.

WORKUP

后处理

  1. stirringThe mixture was stirred at room temperature for 24 hours
  2. filtrationthe precipitate was collected by filtration
  3. dissolutionThe precipitate was dissolved in DMF
  4. filtrationthe insolubles were filtered off
  5. additionThe filtrate containing the DMF-soluble substances
  6. additionwas mixed with ethyl ether
  7. filtrationthe resulting precipitate was collected by filtration
  8. customrecrystallized from a mixture of DMF and ethyl ether